CN107699213A - A kind of preparation method of polyamides amine inhibitors suitable for drilling fluid - Google Patents
A kind of preparation method of polyamides amine inhibitors suitable for drilling fluid Download PDFInfo
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- CN107699213A CN107699213A CN201711076419.5A CN201711076419A CN107699213A CN 107699213 A CN107699213 A CN 107699213A CN 201711076419 A CN201711076419 A CN 201711076419A CN 107699213 A CN107699213 A CN 107699213A
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- drilling fluid
- polyamides amine
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- amine inhibitors
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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
- C08G69/28—Preparatory processes
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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
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/22—Synthetic organic compounds
- C09K8/24—Polymers
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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
- 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
Abstract
The invention discloses a kind of preparation method of the polyamides amine inhibitors suitable for drilling fluid, its step are as follows：A, the substance A weighed up and alcoholic solvent are added in the reactor equipped with electric mixer；B, at ambient temperature, substance B is added dropwise while stirring, after being added dropwise to complete, stirs 30min, then heats to 15 ~ 35 DEG C, stop after reacting 12 ~ 20h；C, mixture is first carried out being evaporated under reduced pressure removing solvent and part unreacting material, is then settled with petroleum ether, the intermediate product of weak yellow liquid is obtained after vacuum drying, is denoted as M；D adds the M Jing Guo simple purification in the reaction kettle body for filling alcoholic solvent, and until completely dissolved, substance C is added drop-wise in reaction system for stirring；E, alcoholic solvent and a small amount of unreacted raw material are removed by being evaporated under reduced pressure, are then extracted in ether, after the completion of vacuum drying obtain wanted synthetic product；The polyamides amine inhibitors prepared using this method have the characteristics that high temperature resistance, inhibition are notable, small to rheology impact.
Description
Technical field
The present invention relates to drilling fluid inhibitor technical field, specifically relates to a kind of polyamide suitable for drilling fluid
The preparation method of inhibitor.
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 suitable for the poly- of drilling fluid
The preparation method of amide inhibitors, the inhibitor prepared using this preparation method is good with conventional water base inorganic agent compatibility, right
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 mineral
The scattered effect of aquation, 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 suitable for drilling fluid, it is characterised in that step is as follows：
A, the substance A weighed up and alcoholic solvent are added in the reactor equipped with electric mixer, stirring makes it fully dissolve；
B, at ambient temperature, it is added dropwise substance B while stirring, the amount ratio of the material of substance A and substance B is 1：6 ~ 8, control is added dropwise
Speed is per second one drop, after being added dropwise to complete, stirs 30min, then heats to 15 ~ 35 DEG C, stops after reacting 12 ~ 20h；
C, mixture is first carried out being evaporated under reduced pressure removing solvent and part unreacting material, then settled with petroleum ether, very
Sky obtains the intermediate product of weak yellow liquid after drying, and is denoted as M；
D adds the M Jing Guo simple purification in the reaction kettle body for filling alcoholic solvent, and until completely dissolved, substance C is dripped for stirring
It is added in reaction system, drips off rear stir about 30min, be warming up to 25 ~ 45 DEG C, reacts 8 ~ 16h；Substance C is with intermediate product M's
The amount ratio of material is 6 ~ 12：1；
E, alcoholic solvent and a small amount of unreacted raw material are removed by being evaporated under reduced pressure, are then extracted in ether, after the completion of it is true
Sky is dried to obtain wanted synthetic product.
Substance A isn≥1；
Substance B isn≥1；
Substance C ism≥1；
Alcoholic solvent nail alcohol, ethanol, normal propyl alcohol, isopropanol, n-butanol or the tert-butyl alcohol.
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℃）Significantly improve, 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：
The acrylate and methanol solvate weighed up is added in the 250mL flasks equipped with electric mixer, stirring makes its abundant
Dissolving.
At ambient temperature, the ethylenediamine necessarily measured is added dropwise while stirring（The amount of the material of acrylate and ethylenediamine
Than position 1：（6~8））, control rate of addition is about a drop per second, and after being added dropwise to complete, stir about 30min, then water-bath raises
15 ~ 35 DEG C, stop after reacting 12 ~ 20h.
Mixture is first carried out being evaporated under reduced pressure to remove solvent and part unreacting material, then settled with petroleum ether,
Obtained after vacuum drying but the intermediate product of yellow liquid, be denoted as M.
By a certain amount of M by simple purification to the three-necked flask for entering the 250mL for filling a certain amount of methanol solvate
In, lasting stirring a period of time, it is sufficiently stirred until completely dissolved, by ethylenediamine（The amount of ethylenediamine and intermediate product M material
Than for（6~12）：1）Gradually it is added drop-wise in reaction system, holding rate of titration is 1 drop/s, drips off rear stir about 30min, is risen
Temperature reacts 8 ~ 16h to 25 ~ 45 DEG C.
Alcoholic solvent and a small amount of unreacted raw material are removed by being evaporated under reduced pressure, is then extracted in ether, after the completion of
Vacuum drying obtains wanted synthetic product.
Embodiment 2：
The 1- M Crs and alcohol solvent weighed up is added in the 250mL flasks equipped with electric mixer, stirring makes it
Fully dissolving.
At ambient temperature, the ethylenediamine necessarily measured is added dropwise while stirring（The material of 1- M Crs and ethylenediamine
Amount than position 1：（6~8））, control rate of addition is about a drop per second, after being added dropwise to complete, stir about 30min, and then water-bath
15 ~ 35 DEG C of rise, stop after reacting 12 ~ 20h.
Mixture is first carried out being evaporated under reduced pressure to remove solvent and part unreacting material, then settled with petroleum ether,
Obtained after vacuum drying but the intermediate product of yellow liquid, be denoted as M.
By a certain amount of M by simple purification to the three-necked flask for entering the 250mL for filling a certain amount of alcohol solvent
In, lasting stirring a period of time, it is sufficiently stirred until completely dissolved, by ethylenediamine（The amount of ethylenediamine and intermediate product M material
Than for（6~12）：1）Gradually it is added drop-wise in reaction system, holding rate of titration is 1 drop/s, drips off rear stir about 30min, is risen
Temperature reacts 8 ~ 16h to 25 ~ 45 DEG C.
Alcoholic solvent and a small amount of unreacted raw material are removed by being evaporated under reduced pressure, is then extracted in ether, after the completion of
Vacuum drying obtains wanted synthetic product.
Embodiment 3：
The 1- M Crs and alcohol solvent weighed up is added in the 250mL flasks equipped with electric mixer, stirring makes it
Fully dissolving.
At ambient temperature, the Putriscine necessarily measured is added dropwise while stirring（1- M Crs and 1,4- fourths two
The amount of the material of amine is than position 1：（6~8））, control rate of addition is about a drop per second, after being added dropwise to complete, stir about 30min,
Then water-bath raises 15 ~ 35 DEG C, stops after reacting 12 ~ 20h.
Mixture is first carried out being evaporated under reduced pressure to remove solvent and part unreacting material, then settled with petroleum ether,
Obtained after vacuum drying but the intermediate product of yellow liquid, be denoted as M.
By a certain amount of M by simple purification to the three-necked flask for entering the 250mL for filling a certain amount of alcohol solvent
In, lasting stirring a period of time, it is sufficiently stirred until completely dissolved, by Putriscine（1,4- butanediamine is with intermediate product M's
The amount ratio of material is（6~12）：1）Gradually it is added drop-wise in reaction system, holding rate of titration is 1 drop/s, drips off rear stir about
30min, 25 ~ 45 DEG C are warming up to, react 8 ~ 16h.
Alcoholic solvent and a small amount of unreacted raw material are removed by being evaporated under reduced pressure, is then extracted in ether, after the completion of
Vacuum drying obtains wanted synthetic 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 79.46%.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 | 55 | 59 | 62 | 65 |
| PV/ mPa.s | 45 | 48 | 53 | 55 |
| YP/Pa | 10 | 11 | 9 | 10 |
| Gel/(10’/10”) | 1.5/4 | 2.5/8 | 3.5/8 | 4/9 |
| FL/HPHT | 7.7 | 8.4 | 8.0 | 9.4 |
| Rolling rate of recovery, % | 73.12 | 88.92 | 87.42 | 89.95 |
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 suitable for drilling fluid, it is characterised in that step is as follows：
A, the substance A weighed up and alcoholic solvent are added in the reactor equipped with electric mixer, stirring makes it fully dissolve；
B, at ambient temperature, it is added dropwise substance B while stirring, the amount ratio of the material of substance A and substance B is 1：6 ~ 8, it is added dropwise to complete
Afterwards, 30min is stirred, then heats to 15 ~ 35 DEG C, is stopped after reacting 12 ~ 20h；
C, mixture is first carried out being evaporated under reduced pressure removing solvent and part unreacting material, then settled with petroleum ether, very
Sky obtains the intermediate product of weak yellow liquid after drying, and is denoted as M；
D adds the M Jing Guo simple purification in the reaction kettle body for filling alcoholic solvent, and until completely dissolved, substance C is dripped for stirring
It is added in reaction system, drips off rear stir about 30min, be warming up to 25 ~ 45 DEG C, reacts 8 ~ 16h；Substance C is with intermediate product M's
The amount ratio of material is 6 ~ 12：1；
E, alcoholic solvent and a small amount of unreacted raw material are removed by being evaporated under reduced pressure, are then extracted in ether, after the completion of it is true
Sky is dried to obtain wanted synthetic product.
A kind of 2. preparation method of polyamides amine inhibitors suitable for drilling fluid according to claim 1, it is characterised in that：
Substance A isn≥1。
A kind of 3. preparation method of polyamides amine inhibitors suitable for drilling fluid according to claim 1, it is characterised in that：
Substance B is n≥1。
A kind of 4. preparation method of polyamides amine inhibitors suitable for drilling fluid according to claim 1, it is characterised in that：
Substance C ism≥1。
A kind of 5. preparation method of polyamides amine inhibitors suitable for drilling fluid according to claim 1, it is characterised in that：
Alcoholic solvent nail alcohol, ethanol, normal propyl alcohol, isopropanol, n-butanol or the tert-butyl alcohol.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109181659A (en) * | 2018-09-10 | 2019-01-11 | 长江大学 | End group is the dendrimer intercalator and preparation method thereof of quaternary ammonium group |
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Application publication date: 20180216 |