CN107652951A - Preparation method of polyamide inhibitor for drilling fluid - Google Patents
Preparation method of polyamide inhibitor for drilling fluid Download PDFInfo
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- CN107652951A CN107652951A CN201711076418.0A CN201711076418A CN107652951A CN 107652951 A CN107652951 A CN 107652951A CN 201711076418 A CN201711076418 A CN 201711076418A CN 107652951 A CN107652951 A CN 107652951A
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- 238000005553 drilling Methods 0.000 title claims abstract description 45
- 239000003112 inhibitor Substances 0.000 title claims abstract description 43
- 239000012530 fluid Substances 0.000 title claims abstract description 38
- 239000004952 Polyamide Substances 0.000 title claims abstract description 27
- 229920002647 polyamide Polymers 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000126 substance Substances 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- OMOVVBIIQSXZSZ-UHFFFAOYSA-N [6-(4-acetyloxy-5,9a-dimethyl-2,7-dioxo-4,5a,6,9-tetrahydro-3h-pyrano[3,4-b]oxepin-5-yl)-5-formyloxy-3-(furan-3-yl)-3a-methyl-7-methylidene-1a,2,3,4,5,6-hexahydroindeno[1,7a-b]oxiren-4-yl] 2-hydroxy-3-methylpentanoate Chemical compound CC12C(OC(=O)C(O)C(C)CC)C(OC=O)C(C3(C)C(CC(=O)OC4(C)COC(=O)CC43)OC(C)=O)C(=C)C32OC3CC1C=1C=COC=1 OMOVVBIIQSXZSZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- 239000013067 intermediate product Substances 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 150000001412 amines Chemical class 0.000 claims description 25
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical group OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 7
- 239000001361 adipic acid Chemical group 0.000 claims description 6
- 235000011037 adipic acid Nutrition 0.000 claims description 6
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical group FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- KBIWNQVZKHSHTI-UHFFFAOYSA-N 4-n,4-n-dimethylbenzene-1,4-diamine;oxalic acid Chemical group OC(=O)C(O)=O.CN(C)C1=CC=C(N)C=C1 KBIWNQVZKHSHTI-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Natural products OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 4
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 229920000305 Nylon 6,10 Polymers 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 11
- 230000002401 inhibitory effect Effects 0.000 abstract description 2
- 238000001704 evaporation Methods 0.000 abstract 1
- 239000011345 viscous material Substances 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 9
- 238000005096 rolling process Methods 0.000 description 9
- 230000005764 inhibitory process Effects 0.000 description 7
- 238000006277 sulfonation reaction Methods 0.000 description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 5
- 230000032683 aging Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000004575 stone Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 239000001103 potassium chloride Substances 0.000 description 3
- 235000011164 potassium chloride Nutrition 0.000 description 3
- 238000004925 denaturation Methods 0.000 description 2
- 230000036425 denaturation Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- -1 ester compound Chemical class 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229920000768 polyamine Polymers 0.000 description 2
- WFIZEGIEIOHZCP-UHFFFAOYSA-M potassium formate Chemical compound [K+].[O-]C=O WFIZEGIEIOHZCP-UHFFFAOYSA-M 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 101000832669 Rattus norvegicus Probable alcohol sulfotransferase Proteins 0.000 description 1
- 241001074085 Scophthalmus aquosus Species 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004807 desolvation Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 210000003746 feather Anatomy 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 244000144992 flock Species 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- ZLMJMSJWJFRBEC-OUBTZVSYSA-N potassium-40 Chemical compound [40K] ZLMJMSJWJFRBEC-OUBTZVSYSA-N 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 239000012453 solvate Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Polyamides (AREA)
Abstract
The invention discloses a preparation method of a polyamide inhibitor for drilling fluid, which comprises the following steps: a. adding a substance A and deionized water into a container, and heating to completely dissolve the substance A; b. adding the substance B into another container, and heating to completely dissolve the substance B; c. slowly pouring the solution of the substance B into the substance A, stirring for 2-3 h, and evaporating the solvent to obtain an intermediate product; d. dissolving a proper amount of intermediate product in deionized water, adding a substance A and a catalyst, and introducing nitrogen to remove oxygen in a system; e. heating to 150-180 ℃, reacting at constant temperature for 1h, heating to 230 ℃, reacting for 2h, vacuumizing to 0.01atm, heating to 270 ℃, removing a heat source after reacting for 4h, keeping vacuum, and cooling to obtain a brown yellow viscous substance, namely a product; the inhibitor prepared by the preparation method has good compatibility with the conventional water-based treating agent, has small influence on the performance of the water-based drilling fluid, and can effectively strengthen the inhibiting capability of the water-based drilling fluid.
Description
Technical field
The present invention relates to drilling fluid inhibitor technical field, specifically relates to a kind of polyamide for drilling fluid and presses down
The preparation method of preparation.
Background technology
When the water-sensitive stratas such as mud stone, shale are crept into using water-base drilling fluid, the easy hydration swelling of subterranean minerals, disperse,
The problems such as so as to cause borehole well instability, drilling fluid rheology unmanageable.So the inhibition of drilling fluid system turns into probing water
The key on quick property stratum.Meanwhile as the shale gas well scope drilled at present constantly expands, quantity is on the increase, wellbore fluid
The inhibition of system becomes a key factor of site safety drilling well.
Conventional water-base drilling fluid inhibitor is mainly sylvite, ammonium salt and amine（Ammonium）Birds of the same feather flock together compound inhibitors, although tool
There is certain inhibition, but it is limited for mud stone scattered by force, inhibition.And in actual application, if can not be high
Effect suppresses the scattered of mud stone, the surface of clay after disperseing can rapid adsorption inhibitor, under causing the effective content of inhibitor rapid
Drop, so as to cause the rejection ability of drilling fluid to decline rapidly.
Publication No. CN102504065A, publication date disclose a kind of brill for the Chinese patent literature on June 20th, 2012
Well liquid polyamine inhibitor and preparation method thereof；Initiator and acid-binding agent are placed in reactor, under normal pressure and nitrogen protection,
Sulfonyl agent is added dropwise into reactor, carries out sulphur esterification, the reaction time is 10~12 hours, and sulphur esterification temperature is 0~30
DEG C, reactant is filtered, filtrate is soluble in water, after static split-phase, a layer liquid is removed, vacuum distillation goes to remove water, and obtains end sulphur
Base ester compound；End sulfo group carboxylate is added drop-wise in the reactor equipped with aminating agent and precipitating reagent and carries out aminating reaction, reaction 2~
3 hours, amination temperature was 70~90 DEG C, and product is filtered, and is evaporated under reduced pressure desolvation, obtains polyamine inhibitor；The additive is fitted
It for a variety of water-base drilling fluids, can be good at controlling the aquation of mud shale to disperse, effectively reduce because shale hydration disperses
The problems such as drilling fluid brought thickens, property of drilling fluid deteriorates, to realize that safe and efficient drilling well provides certain guarantee.
But be the conventional inhibitor of representative due to limited sorption capacity using above-mentioned patent document, frequently result in high temperature
Lower generation desorption, so as to cause to lose inhibitory action under high temperature.So to solve the problems, such as the suppression of drilling fluid, it is necessary to research and develop
Specifically for the water-base drilling fluid high temperature resistance inhibitor of water-sensitive formation drilling well, effectively reduce borehole well instability and landwaste aquation disperseed,
Meet the technology needs of live water-sensitive strata high-quality and safety rapid drilling, improve exploration and development benefit.
The content of the invention
It is contemplated that the defects of present in above-mentioned prior art and deficiency, there is provided a kind of polyamides for drilling fluid
The preparation method of amine inhibitors, the inhibitor prepared using this preparation method is good with conventional water base inorganic agent compatibility, to water
Base drilling fluid performance impact is small, and the rejection ability of energy efficient hardening water-base drilling fluid, reaches and suppresses water-sensitive formation fossil water
Change scattered effect, so as to reduce drilling cost, ensure drilling safety and speed.
The present invention is realized by using following technical proposals：
The preparation method of a kind of polyamides amine inhibitors for drilling fluid, it is characterised in that step is as follows：
A, substance A and deionized water are added in a reservoir, and being slowly heated under the conditions of not higher than 55 DEG C is completely dissolved substance A；
B, substance B is added in another container, the ratio of the amount of the material of substance B and substance A is 1 ~ 1.2：1, and alcoholic solvent is added,
Heated under the conditions of not higher than 50 DEG C, be completely dissolved substance B；
C, in the case where rapidly stirring, the solution of substance B is poured slowly into substance A while hot, 2 ~ 3h is stirred, steams solvent, in being
Between product；
D, appropriate intermediate product is taken to be dissolved in deionized water, additive A, catalyst, the addition of catalyst is substance A
1Wt%, the oxygen being passed through in nitrogen removal system；
E, 150 ~ 180 DEG C, isothermal reaction 1h are heated to, then is warming up to 230 DEG C, 2h is reacted, vacuumizes 0.01atm, is heated up
270 DEG C, thermal source is removed in reaction 4h recession, keeps vacuum, cooling, brown color thick substances are product；
Substance A is ethylenediamine, Putriscine, one kind in hexamethylene diamine；
Substance B is ethanedioic acid, adipic acid, one kind in the binary acid such as decanedioic acid；
Catalyst is sodium hypophosphite；
Alcoholic solvent nail alcohol, ethanol or isopropanol.
Compared with prior art, what the present invention was reached has the beneficial effect that：
By the checking of embodiment, it can learn that it has the following technical effect that：
1st, polyamides amine inhibitors, mud shale landwaste rolling rate of recovery can be made（150℃）Up to 75.23%, there is good suppression to make
With the rheological characteristic of drilling fluid system and the stabilization of leak-off wall building property can be kept；
2nd, polyamides amine inhibitors and conventional treatment agent compatibility are good, influence little, drilling well liquid stream to the overall performance of drilling fluid
Denaturation, leak-off wave making machine are substantially unaffected；
3rd, polyamides amine inhibitors have good temperature resistance, and temperature resistance is up to 150 DEG C.
In summary, using this method prepare polyamides amine inhibitors have high temperature resistance, inhibition significantly, to rheological characteristic
The features such as small is influenceed, suitable for various water base drilling fluid systems.It can not only prevent that water-sensitive formation clay mineral aquation is scattered, swollen
It borehole well instability problem caused by swollen, can also effectively stablize the rheological characteristic of drilling fluid system, avoid generation performance out of control.In addition,
For the inhibitor in drilling fluid system, for dosage with safeguarding that dosage is small, expense is low, can significantly save drilling fluid cost.With multiple
The continuous expansion of drilling well scale under miscellaneous geological conditions, the polyamides amine inhibitors market application foreground is wide, has good economy
Benefit.
Embodiment
Embodiment 1：
A certain amount of ethylenediamine and deionized water are added in a reservoir, are slowly heated（Not higher than 55 DEG C）It is allowed to be completely dissolved；
Ethanedioic acid is added in another container（With the ratio position of the amount of the material of ethylenediamine（1~1.2）：1）, add a certain amount of first
Alcoholic solvent, heating（Not higher than 50 DEG C）, it is allowed to be completely dissolved；
In the case where rapidly stirring, the solution of ethanedioic acid is poured slowly into ethylenediamine while hot, 2 ~ 3h is stirred, steams solvent, in being
Between product.
Take a certain amount of intermediate product to be dissolved in deionized water, add a small amount of ethylenediamine, Sodium Hypophosphite catalyst（For ethylenediamine
1Wt%）, it is passed through nitrogen bubble 3min, the oxygen in removal system；
150 ~ 180 DEG C, isothermal reaction 1h are heated to, then is warming up to 230 DEG C, reacts 2h, vacuumizes 0.01atm, heating 270
DEG C, thermal source is removed in reaction 4h recession, keeps vacuum, cooling, brown color thick substances are product.
Embodiment 2：
A certain amount of Putriscine and deionized water are added in a reservoir, are slowly heated（Not higher than 55 DEG C）It is allowed to completely molten
Solution；
Adipic acid is added in another container（With the ratio position of the amount of the material of Putriscine（1~1.2）：1）, add a certain amount of
Methanol solvate, heating（Not higher than 50 DEG C）, it is allowed to be completely dissolved；
In the case where rapidly stirring, the solution of adipic acid is poured slowly into Putriscine while hot, 2 ~ 3h is stirred, steams solvent, i.e.,
For intermediate product.
Take a certain amount of intermediate product to be dissolved in deionized water, add a small amount of Putriscine, Sodium Hypophosphite catalyst（For 1,
The 1Wt% of 4- butanediamine）, it is passed through nitrogen bubble 3min, the oxygen in removal system；
150 ~ 180 DEG C, isothermal reaction 1h are heated to, then is warming up to 230 DEG C, reacts 2h, vacuumizes 0.01atm, heating 270
DEG C, thermal source is removed in reaction 4h recession, keeps vacuum, cooling, brown color thick substances are product.
Embodiment 3：
A certain amount of hexamethylene diamine and deionized water are added in a reservoir, are slowly heated（Not higher than 55 DEG C）It is allowed to be completely dissolved；
Adipic acid is added in another container（With the ratio position of the amount of the material of hexamethylene diamine（1~1.2）：1）, add a certain amount of first
Alcoholic solvent, heating（Not higher than 50 DEG C）, it is allowed to be completely dissolved；
In the case where rapidly stirring, the solution of adipic acid is poured slowly into hexamethylene diamine while hot, 2 ~ 3h is stirred, steams solvent, in being
Between product.
Take a certain amount of intermediate product to be dissolved in deionized water, add a small amount of hexamethylene diamine, Sodium Hypophosphite catalyst（For Isosorbide-5-Nitrae-fourth
The 1Wt% of diamines）, it is passed through nitrogen bubble 3min, the oxygen in removal system；
150 ~ 180 DEG C, isothermal reaction 1h are heated to, then is warming up to 230 DEG C, reacts 2h, vacuumizes 0.01atm, heating 270
DEG C, thermal source is removed in reaction 4h recession, keeps vacuum, cooling, brown color thick substances are product.
Embodiment method of evaluating performance
1st, polyamides amine inhibitors rolling rate of recovery is tested
4 parts of 350mL distilled water are taken, wherein three parts of polyamides amine inhibitors for being separately added into 1%（Embodiment 1）, 7% conventional inhibitor
Potassium chloride and 40% conventional inhibitor potassium formate, in low-speed agitator（1000rpm/min）Upper stirring 10min.By four parts of liquid
Body is poured into ageing can, then is separately added into 50g mud shale landwaste.The rolling rate of recovery of four parts of liquid is determined at 150 DEG C, as a result
Such as table 2：
The polyamides amine inhibitors of table 1 contrast with other conventional inhibitor mud shale landwaste rolling rate of recoveries
From table 1, the landwaste rolling rate of recovery of clear water is only 15.64%, and the rolling rate of recovery of the potassium chloride of conventional inhibitor 7%
For 27.52%, 40% potassium formate is 58.42%.And 1% polyamides amine inhibitors are only added, landwaste rolling rate of recovery is 75.23%.It is real
Test result to show, polyamides amine inhibitors have the excellent ability for suppressing hydration of mud stone and disperseing under 150 DEG C of environment.
2nd, influence of the polyamides amine inhibitors to drilling fluid system combination property
Influence of the polyamides amine inhibitors of table 2 to drilling fluid system combination property
| System forms | Basic sulfonation system | Sulfonation system -1 | Sulfonation system -2 | Sulfonation system -3 |
| Bentonite, % | 2 | 2 | 2 | 2 |
| Embodiment 2#, % | 1 | 0.5 | 0 | |
| Embodiment 3#, % | 0 | 0.5 | 1 | |
| SMP-2,% | 4 | 4 | 4 | 4 |
| SPNH,% | 2 | 2 | 2 | 2 |
| RSTF,% | 2 | 2 | 2 | 2 |
| Anti-seize lubricant, % | 1 | 1 | 1 | 1 |
| Performance | 150 DEG C of aging 16h | 150 DEG C of aging 16h | 150 DEG C of aging 16h | 150 DEG C of aging 16h |
| Density, g/ml | 2.1 | 2.1 | 2.1 | 2.1 |
| AV/ mPa.s | 59 | 64 | 65 | 68 |
| PV/ mPa.s | 47 | 55 | 54 | 57 |
| YP/Pa | 12 | 9 | 11 | 11 |
| Gel/(10’/10”) | 1.5/5 | 2/6 | 3/8 | 4/9 |
| FL/HPHT | 8.2 | 8.0 | 8.5 | 8.3 |
| Rolling rate of recovery, % | 74.32 | 80.54 | 84.70 | 84.52 |
As can be seen from Table 2, after adding polyamides amine inhibitors in Common sulfonation system, rolling rate of recovery is significantly raised, indicates
Polyamides amine inhibitors have good inhibition, and the inhibition of drilling fluid can be substantially improved.With the stream of basic sulfonation system
Denaturation is compared with leak-off wave making machine, and after adding polyamides amine inhibitors, the leak-off wave making machine of drilling fluid system does not have significant change, and
Rheological characteristic slightly rises, but unobvious, illustrates that polyamides amine inhibitors influence on the rheological characteristic of drilling fluid system with leak-off wave making machine
Less, the inhibitor has good compatibility.
Claims (5)
1. the preparation method of a kind of polyamides amine inhibitors for drilling fluid, it is characterised in that step is as follows：
A, substance A and deionized water are added in a reservoir, and being heated under the conditions of not higher than 55 DEG C is completely dissolved substance A；
B, substance B is added in another container, the ratio of the amount of the material of substance B and substance A is 1 ~ 1.2：1, and alcoholic solvent is added,
Heated under the conditions of not higher than 50 DEG C, be completely dissolved substance B；
C, the solution of substance B is poured into substance A, stirs 2 ~ 3h, steam solvent, as intermediate product；
D, appropriate intermediate product is taken to be dissolved in deionized water, additive A, catalyst, the addition of catalyst is substance A
1Wt%, the oxygen being passed through in nitrogen removal system；
E, 150 ~ 180 DEG C, isothermal reaction 1h are heated to, then is warming up to 230 DEG C, 2h is reacted, vacuumizes 0.01atm, is heated up
270 DEG C, thermal source is removed in reaction 4h recession, keeps vacuum, cooling, brown color thick substances are product.
A kind of 2. preparation method of polyamides amine inhibitors for drilling fluid according to claim 1, it is characterised in that：Thing
Matter A is ethylenediamine, Putriscine, one kind in hexamethylene diamine.
A kind of 3. preparation method of polyamides amine inhibitors for drilling fluid according to claim 1, it is characterised in that：Thing
Matter B is ethanedioic acid, adipic acid, one kind in the binary acid such as decanedioic acid.
A kind of 4. preparation method of polyamides amine inhibitors for drilling fluid according to claim 1, it is characterised in that：Urge
Agent is sodium hypophosphite.
A kind of 5. preparation method of polyamides amine inhibitors for drilling fluid according to claim 1, it is characterised in that：Alcohol
Solvent nail alcohol, ethanol or isopropanol.
Priority Applications (1)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111320972A (en) * | 2018-12-13 | 2020-06-23 | 中石化石油工程技术服务有限公司 | Amido chitosan, preparation method thereof and drilling fluid |
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Application publication date: 20180202 |