CN105277657B - The assay method of drilling fluid organic agent absorption property - Google Patents
The assay method of drilling fluid organic agent absorption property Download PDFInfo
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- CN105277657B CN105277657B CN201410299336.2A CN201410299336A CN105277657B CN 105277657 B CN105277657 B CN 105277657B CN 201410299336 A CN201410299336 A CN 201410299336A CN 105277657 B CN105277657 B CN 105277657B
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- 238000005553 drilling Methods 0.000 title claims abstract description 146
- 239000012530 fluid Substances 0.000 title claims abstract description 114
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 33
- 238000003556 assay method Methods 0.000 title claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 113
- 239000004927 clay Substances 0.000 claims abstract description 70
- 229910052570 clay Inorganic materials 0.000 claims abstract description 70
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 239000000706 filtrate Substances 0.000 claims description 57
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 50
- 229910052799 carbon Inorganic materials 0.000 claims description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 41
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- 239000006194 liquid suspension Substances 0.000 claims description 25
- 239000012528 membrane Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- 239000010703 silicon Substances 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 210000004369 Blood Anatomy 0.000 claims description 4
- 239000008280 blood Substances 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 239000003112 inhibitor Substances 0.000 claims description 3
- 230000002401 inhibitory effect Effects 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 239000000654 additive Substances 0.000 abstract description 48
- 230000000996 additive Effects 0.000 abstract description 48
- 238000011156 evaluation Methods 0.000 abstract description 12
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- 238000005457 optimization Methods 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 description 17
- VXMKYRQZQXVKGB-CWWHNZPOSA-N Tannin Chemical compound O([C@H]1[C@H]([C@@H]2OC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)O[C@H]([C@H]2O)O1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 VXMKYRQZQXVKGB-CWWHNZPOSA-N 0.000 description 13
- 239000007788 liquid Substances 0.000 description 13
- 229920001864 tannin Polymers 0.000 description 13
- 235000018553 tannin Nutrition 0.000 description 13
- 239000001648 tannin Substances 0.000 description 13
- 238000006277 sulfonation reaction Methods 0.000 description 11
- 239000006228 supernatant Substances 0.000 description 9
- HRPVXLWXLXDGHG-UHFFFAOYSA-N acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- 239000000178 monomer Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 238000011085 pressure filtration Methods 0.000 description 5
- 239000002689 soil Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 238000002798 spectrophotometry method Methods 0.000 description 4
- 241001074085 Scophthalmus aquosus Species 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 230000003287 optical Effects 0.000 description 3
- 125000001477 organic nitrogen group Chemical group 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000001603 reducing Effects 0.000 description 3
- 239000003638 reducing agent Substances 0.000 description 3
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- 238000003786 synthesis reaction Methods 0.000 description 3
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- 229910000604 Ferrochrome Inorganic materials 0.000 description 2
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- 241000255964 Pieridae Species 0.000 description 2
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
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- 238000010276 construction Methods 0.000 description 2
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000005375 photometry Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
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- 239000011780 sodium chloride Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- CDRBDEPNXGRWGI-UHFFFAOYSA-N 2-methylprop-2-enoyloxyazanium Chemical compound CC(=C)C(=O)O[NH3+] CDRBDEPNXGRWGI-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
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- 238000010790 dilution Methods 0.000 description 1
- KARVSHNNUWMXFO-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane;hydrate Chemical compound O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O KARVSHNNUWMXFO-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
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- 229910052901 montmorillonite Inorganic materials 0.000 description 1
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- AJURYMCOXVKKFB-UHFFFAOYSA-M trimethyl(3-prop-2-enoyloxypropyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCCOC(=O)C=C AJURYMCOXVKKFB-UHFFFAOYSA-M 0.000 description 1
- SZYJELPVAFJOGJ-UHFFFAOYSA-N trimethylamine hydrochloride Chemical compound Cl.CN(C)C SZYJELPVAFJOGJ-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention provides a kind of assay method of additive for drilling fluid absorption property, particularly provide a kind of assay method of additive for drilling fluid high temperature adsorption performance, this method carries out heat filtering using the drilling fluid system comprising inorganic agent, such as leak-off back pressure under the high temperature conditions, liquid phase in acquisition system, the quality of additive for drilling fluid not to be adsorbed under hot conditions is calculated by determining the percentage composition of inorganic agent characteristic element in liquid phase, and then calculate adsorbance of the inorganic agent in drilling fluid on clay under hot conditions, realize the evaluation to additive for drilling fluid absorption property under the high temperature conditions.It is the assay method science, accurate, the evaluation of the high temperature adsorption performance for the drilling fluid organic agent that is particularly suitable for use in, be Exact Design and OPTIMIZATION OF DRILLING FLUID inorganic agent molecular structure, rational drilling fluid composition offer technical support is provided.
Description
Technical field
The present invention relates to the performance evaluation field of additive for drilling fluid, and in particular to a kind of drilling fluid organic agent absorption
The assay method of performance, more particularly to a kind of assay method of drilling fluid organic agent high temperature adsorption performance.
Background technology
Drilling fluid is commonly called as mud, is a kind of fluid being formulated by various raw material and chemical addition agent, in drilling well
Cheng Zhong, play suspension and cutting carring, lubrication drill bit, stabilizing borehole and equilibrium strata pressure and transmit the work(such as hydrodynamic force
Can, it is drilling safety and the important leverage for protecting oil and gas reservoir.In Process of Oil Well Drilling, in order to adjust the performance of drilling fluid,
Ensure that the used chemical products that are smoothed out of drillng operation are referred to as drilling fluid chemicals, i.e. additive for drilling fluid.Drilling well
Important component of the liquid inorganic agent as drilling fluid, very important work is played on property of drilling fluid safeguarding and improving
With.At present, China's additive for drilling fluid has developed to 18 major classes, hundreds of varieties, nearly 300,000 tons of annual production, and the product of inorganic agent
Kind increasingly becomes more meticulous.At present, the additive for drilling fluid overwhelming majority used in field of oil drilling is organic agent.
Within one period from now on, the situation that drilling engineering faces is the probing problem of deep-well, ultradeep well, and these wells
An important feature be exactly that bottom hole temperature (BHT) is higher, it is necessary to add the inorganic agent of high temperature resistance to ensure during wellbore construction
Wellbore construction is smoothed out, and this just needs the R＆D worker of inorganic agent to develop the Deal With Drilling Fluid suitable for high temperature deep well
Agent.
It is well known that the inorganic agent of the overwhelming majority plays a role in drilling fluid and all realized by adsorbing, especially
It is even more so for organic agent.For example, fluid loss additive forms hydration shell by the absorption in surface of clay, cause viscous
Native surface zeta potential rise, clay particle is prevented to maintain fine grain content in drilling fluid because collision produces coalescence, reduce filter
Vector；Thinner forms hydration shell by the absorption in clay end face, break and weaken between clay particle by end-face and
End-end connects the grid structure to be formed, so as to reach the purpose for reducing viscosity；The absorption base that organic inhibitor passes through molecular surface
Group grabs adsorption site, reduces hydration swelling, reach and suppress what clay aquation was disperseed prior to Water Molecular Adsorption to surface of clay
Purpose.As can be seen here, the absorption property of research and appraisal drilling liquid inorganic agent, MOLECULE DESIGN to auxiliary drill well liquid inorganic agent,
Probe into molecular mechanisms of action, preferred process agent kind and OPTIMIZATION OF DRILLING FLUID system formulation etc. have important theory significance and
Actual application value.Therefore, when carrying out additive for drilling fluid new-product development, it is necessary to which emphasis considers the suction of additive for drilling fluid
Attached performance, the additive for drilling fluid of high temperature resistance are no exception.
However, at present for inorganic agent under the high temperature conditions absorption property evaluation method mostly be to use loss method and extinction
Photometry.Loss method, such as Shandong University's master thesis in 2008《The synthesis of heat-resistant polymer filtrate reducer for drilling fluid and
Study on mechanism》It is described, the clay dispersion system centrifuging and taking supernatant containing fluid loss additive of adsorption equilibrium is up to, is diluted,
The content of the organic carbon in organic carbon determination instrument measure dilution is recycled, so as to know the carbon content in supernatant；Then, then
Subtracted with the original addition of fluid loss additive in supernatant not by the amount of the fluid loss additive of adsorption by clay, that is, obtain adsorbed drop
The amount of fluid loss agents.But the experimentation that is measured of centrifuging and taking supernatant involved in the assay method by experiment condition,
Instrument and human factor have a great influence, that is, fail with centrifugation and settle be suspended in supernatant a small amount of be adsorbed with inorganic agent
Clay particle the accuracy of measurement result will necessarily be had an impact；Even more noteworthy, the whole mistake of the assay method
Cheng Jun is carried out under normal temperature condition, and measurement result is only able to display under the additive for drilling fluid normal temperature condition in surface of clay
Adsorbance, inorganic agent, will necessarily be by determining instrument use condition in the adsorbance of surface of clay when measure is higher than 100 DEG C
Limitation.Therefore, this method is not particularly suited for evaluating the absorption property of inorganic agent under the high temperature conditions.For additive for drilling fluid height
The evaluation method of warm absorption property, Shandong University's master thesis in 2010《The synthesis of heat-resistant salt-resistant fluid loss additive and with illiteracy
Take off the repercussion study of soil》Loss method is improved, the clay dispersion system that will contain inorganic agent is placed in HTHP
Heated in reactor, cooled down after reaching adsorption equilibrium, centrifuged, take supernatant, determine organic carbon content, then again to absorption
Amount is calculated.But this method have ignored it is cold after the clay dispersion system of inorganic agent is taken out from high temp roller furnace
But during, the part inorganic agent in system can adsorb in clay particle surface again with the reduction of temperature, so as to cause often
The adsorbance determined under the conditions of temperature can not truly reflect that inorganic agent is in the adsorbance of surface of clay under the high temperature conditions.Therefore,
The loss method still has certain defect for the absorption property of appraisal drilling liquid inorganic agent under the high temperature conditions.
Absorption photometry is also a kind of common method of appraisal drilling liquid inorganic agent, sees nineteen eighty-two earliest《Southwestern oil
Institute's journal》In《Adsorbances of the spectrophotometry SMP on soil is removed》One text.This method is to be based on bright Mooreis law,
Using the relation between optical density and concentration, using spectrophotometry additive for drilling fluid surface of clay absorption
Amount.Specifically, this method determines optical density at different wave length, obtains concentration of standard solution-suction using distilled water as reference solution
Photometric standard curve.Inorganic agent-clay dispersion the system for being up to adsorption equilibrium carries out centrifugal solid-liquid separation, by determining liquid phase
In optical density, the amount of inorganic agent in liquid phase is calculated further according to concentration of standard solution-absorbance standard curve, and then inhaled
The amount for the inorganic agent being attached on clay.But when processing agent concentration is higher, light adsorption curve can bend, and influence to determine
As a result accuracy.If inorganic agent is coloring treatment agent, being retained in colored composition small in supernatant can also make light absorption bent
Larger skew occurs for line, so as to cause measurement result inaccurate.In addition, the evaluation method is currently only used for evaluating under normal temperature condition
Absorption property of the inorganic agent on clay.
The content of the invention
The invention aims to overcome deficiency of the prior art and defect as described above, there is provided a kind of drilling fluid
The evaluation method of organic agent absorption property, it can be realized to drilling fluid organic agent under hot conditions on clay
Adsorbance carries out Accurate Determining, truly reflects the absorption property of drilling fluid organic agent under the high temperature conditions.
According to the present invention, there is provided a kind of assay method of drilling fluid organic agent absorption property, comprise the following steps：
A) drilling fluid organic agent, clay and water are mixed, obtains drilling well liquid suspensions；B) drilling well liquid suspensions are subjected to hot mistake
Filter；C) content of the carbon and/or nitrogen in filtrate is determined.In method provided by the invention, the heat filtering can be with
By means of the existing arbitrary equipment for the heat filtering that can realize additive for drilling fluid to be measured.Such equipment for example can be bag
The equipment for including the unit that can accommodate additive for drilling fluid to be measured, filter element and temperature-controlled member, it can be seal or non-close
Closing property.As described above, in the prior art, people to the evaluation method of the high temperature adsorption performance of drilling fluid organic agent due to
There is certain defect and larger deviation brought to evaluation result in its used technological means, and the present inventor passes through
Take the measure of heat filtering so that the measurement result obtained can truly reflect drilling fluid organic agent in hot conditions
Under absorption property.
In a preferred embodiment, the step b) includes：Step b1) the drilling well liquid suspensions are added to height
In warm high pressure filtration device, predetermined temperature is warming up to；B2) after reaction to the scheduled time, collect in high pressure high temperature filter tester through filter
The filtrate of film.High pressure high temperature filter tester, it is dedicated for measure drilling fluid (mud) in oil exploitation research field as its name suggests
Filter loss instrument.High pressure high temperature filter tester is mainly by the fluid-containing pot equipped with filter membrane, sealing system, temperature control and pressure charging system group
Into.The instrument can simulate downhole temperature and pressure difference, and wherein filter membrane serves as the borehole wall of simulation.Make in the routine of high pressure high temperature filter tester
In, prepare liquid is injected into fluid-containing pot, and temperature and pressure are adjusted into setting value, design temperature setting value to be achieved or pre- timing
Between after, open the filtrate discharge valve on filtration device, make the sealing system of filtration device is inside and outside to form pressure difference, collect filtrate and simultaneously measure
Its volume, you can measure filter loss, can also carry out the research such as intensity to filter cake if necessary.However, the present inventor is but
High pressure high temperature filter tester is dexterously applied in the method for the absorption property that the present invention is used for appraisal drilling liquid inorganic agent, not only
The defects of failing to carry out heat filtering in existing evaluation method is overcome, also further allows the heat filtering process very
Easily realize.High pressure high temperature filter tester used in the present invention can be existing or current on the market any one is high
Warm high pressure filtration device, as long as the purpose of the present invention can be realized.
In method provided by the present invention, heat filtering temperature and step b1 in step b)) described in pre- constant temperature
Degree and step b2) described in the scheduled time can be needed according to specific experiment and application to determine.For temperature, such as can
To be normal temperature or high temperature higher than 100 DEG C.However, a prominent advantage as the present invention, the invention provides
A kind of assay method of drilling fluid organic agent high temperature adsorption performance, the high temperature is in view of high pressure high temperature filter tester highest
Under the conditions of operating temperature and filter membrane temperature in use, select and be embodied in the design temperature as needed.Therefore, setting temperature
Degree can be set to such as 85-260 DEG C, such as 100-220 DEG C, in another example 130-180 DEG C.The temperature of this namely heat filtering.Phase
Should be in the practical service environment of drilling fluid organic agent, i.e., the temperature on the stratum that drilling fluid is reached is (general in drilling process
No more than 220 DEG C), in the certain preferred embodiments of the present invention, predetermined temperature is 100-220 DEG C.For time, a side
Face, method of the invention can determine the adsorbance size of any time, depending on needs；On the other hand, can adopt
The Dynamic Adsorption rule of certain organic agent is studied with the method for the present invention, so that after time of equilibrium adsorption is determined,
The adsorbance of additive for drilling fluid is measured during to reaching adsorption equilibrium.In method provided by the invention, pressure equally may be used
To set as needed, such as 0.68-8.5MPa, preferably commonly used in the art for measure drilling fluid organic agent performance
The 3.5MPa of test.
Certainly, it is readily appreciated that, the drilling fluid organic agent high temperature adsorption although method provided by the invention is particularly suitable for use in
The test of performance, but on the other hand, can be by step b1) in predetermined temperature be set to normal temperature (such as 20 DEG C), it is so same
Sample can obtain the accurate result of the absorption property of drilling fluid organic agent at normal temperatures.On this point, invention of the invention
People have also been made corresponding experiment to verify, obtained result and the AAS (spectrophotometry provided using Yan Jie
Adsorbances of the SMP on soil is removed, Southwest Petroleum Institute journal, phase nineteen eighty-two the 1st) result that is measured is suitable.
All realized, therefore handled by adsorbing because current most inorganic agent plays a role in drilling fluid
The screening of agent composition and the optimization of drilling fluid composition largely only need to refer to absorption of the inorganic agent composition on clay
Performance, or completed with reference to the comparison of absorption property of multiple alternative inorganic agent compositions on clay.Therefore, in the present invention
Method in, it is only necessary to investigate adsorbance of the additive for drilling fluid on clay.That is, in the measure drilling fluid of the present invention
In the method for organic agent high temperature adsorption performance, without being measured using complicated drilling fluid system, and it need to only use viscous
Base fluid of the mixture of soil and water as measure.
In addition, the present inventor, it is considered that carbon is the characteristic element of all drilling fluid organic agents, nitrogen is first
Element is the characteristic element of most of drilling fluid organic agents, therefore is obtained by directly determining the content of carbon and/or nitrogen
Know the amount of drilling fluid organic agent.Similarly, element silicon is the characteristic element of clay.Also, generally used in this area
Clay in and do not contain carbon and nitrogen.Therefore, in the method for the invention, need to only determine carbon in filtrate and/or
The content of nitrogen, you can know the amount of inorganic agent not to be adsorbed, and then learn the amount of adsorbed inorganic agent.Easily reason
Solution, it is to contain nitrogen in the drilling fluid organic agent when the method for the present invention only measure nitrogen element content in step c)
The situation of element.
Drilling fluid organic agent of the present invention can be any in various organic agents commonly used in the art
It is one or more.The drilling fluid organic agent for example can be mentioned that thinner, fluid loss additive, coating agent, tackifier, flocculation
Agent, surfactant, inhibitor etc..Because the present invention is using system is simply determined, the measure system of complicated component is avoided,
Therefore only need to determine the carbon and/or nitrogen in filtrate, you can obtain the adsorbance of inorganic agent, method is simple, accurate
Degree is high, cost is low.Further, since the additive for drilling fluid overwhelming majority used in field of oil drilling is organic place at present
Agent is managed, i.e., all contains characteristic element carbon and/or nitrogen, so method provided by the invention is applied widely, it is practical.
Importantly, the method according to the invention overcomes the conventional determining method of additive for drilling fluid absorption property not
The problem of adsorbance for the inorganic agent that can truly reflect under high temperature adsorption balance.The present invention is not directed to the cooling of drilling well liquid suspensions
Process, but the liquid phase (i.e. filtrate) obtained by heat filtering, the content that ensure that the inorganic agent in liquid phase (i.e. filtrate) are
Under hot conditions in drilling well liquid suspensions liquid phase inorganic agent content, ensure that test result is true and reliable.Specifically, it is of the invention
Working environment of the drilling fluid in oil field stratum dexterously is simulated using high pressure high temperature filter tester, and works as the organic place of drilling fluid
Agent is managed after certain adsorption time, such as after reaching adsorption equilibrium, is filtered under high-temperature and high-pressure conditions, therefore this
The method of invention can truly reflect absorption property of the drilling fluid organic agent in actual job.
In one embodiment of the invention, the above method is additionally included in the step c-1 before step c))：Measure filter
The content of element silicon in liquid.Step c-1) it can also specifically include when the silicon content in filtrate is not zero, by described in
Filter membrane replacing is the smaller filter membrane in aperture and repeat step a)~c-1), until the silicon content in filtrate is zero.This process
Actually select the filter membrane in a suitable high pressure high temperature filter tester, it is ensured that clay in drilling fluid is adsorbed with processing
The clay of agent does not enter into filtrate, further ensures the accuracy of test result.Therefore, compared to directly right in the prior art
Filtrate, which carries out absorbance measurement or carbon measure, measurement of the invention, has higher accuracy and reliability.It is once suitable
Filter membrane aperture be chosen after, then need not each time test in be required for reselecting.
Carbon in filtrate can be measured using organic carbon analyzer；Nitrogen can use organic blood urea/nitrogen analyzer
It is measured；Element silicon can be measured using common elemental analyser, such as inductively coupled plasma atomic emission
Instrument (ICP-OES) etc..
Method provided by the invention also include in the cubage filtrate of carbon in filtrate or nitrogen not by
The quality of the drilling fluid organic agent of absorption, and then calculate and obtain adsorbance of the drilling fluid organic agent on clay.
Specifically, adsorbance of the drilling fluid organic agent on clay is calculated by Formulas I：
Wherein, KAdsorbanceAdsorbance of-drilling fluid the organic agent on clay, mgg-1；
mClayThe quality of clay in-drilling well liquid suspensions, g；
mInorganic agentThe quality of drilling fluid organic agent in-drilling well liquid suspensions, g；
mFiltrateThe quality of-filtrate, g；
The weight/mass percentage composition of carbon or nitrogen in P- filtrates, %；
The Theoretical Mass percentage composition of L- carbons or nitrogen in drilling fluid organic process agent molecule, %.
It is readily appreciated that, when P refers to the weight/mass percentage composition of the carbon in filtrate, L accordingly refers to carbon and bored
Theoretical Mass percentage composition in well liquid organic process agent molecule；When P refers to the weight/mass percentage composition of the nitrogen in filtrate,
L accordingly refers to Theoretical Mass percentage composition of the nitrogen in drilling fluid organic process agent molecule.
The assay method of drilling fluid organic agent absorption property provided by the invention can be beneficially based on high temperature filtration,
Using the leak-off back pressure under the high temperature conditions of the drilling fluid system comprising inorganic agent, the liquid phase (i.e. filtrate) in acquisition system, pass through
The percentage composition of the characteristic element of inorganic agent calculates additive for drilling fluid not to be adsorbed under hot conditions in measure filtrate
Quality, and then adsorbance of the inorganic agent in drilling fluid on clay under hot conditions is calculated, realize to drilling fluid organic process
The evaluation of agent absorption property under the high temperature conditions.The assay method science, accurate, be particularly suitable for use in organic drilling fluid organic process
The evaluation of the high temperature adsorption performance of agent, accurately to determine that rational drilling fluid composition provides technical support.
Embodiment
Below will by specific embodiment, the present invention will be further described, but the scope of the present invention is not limited to this.
Embodiment 1
The measure of high temperature (150 DEG C) adsorbance of thinner sulfonation tannin in the weight % of argillaceous 4.0 drilling fluid
Specific experiment step is as follows：
1) sulfonation tannin, clay and water are sufficiently mixed in proportion, are configured to the brill that sulfonation tannin concentration is 1.0 weight %
Well liquid suspension, wherein clay weight account for the 4.0% of clay and water gross weight.
2) apparent viscosity (AV) and yield value (YP) of above-mentioned drilling well liquid suspensions are determined, the results are shown in Table 1.
3) drilling well liquid suspensions are added in high pressure high temperature filter tester, are warming up to 150 DEG C, pressure is arranged to 3.5MPa.
4) after 1.0 hours, the back-pressure valve on high pressure high temperature filter tester is opened, casts out filtrate obtained by spurt loss, is collected stable
The filtrate of high pressure high temperature filter tester bottom filter membrane is passed through under the conditions of leak-off, records filtrate quality.
5) ICP-OES is utilized, determines the content of element silicon in filtrate, measurement result shows that its value is not zero；By step 4)
In be arranged on the filter membrane replacing of high pressure high temperature filter tester bottom into the smaller filter membrane of filter opening, repeat experimental procedure 1)~4), again
The filtrate of high pressure high temperature filter tester bottom filter membrane is passed through under the conditions of the stable leak-off of acquisition, records the quality of the filtrate of this acquisition.
Using organic carbon analyzer, the content of carbon in filtrate is determined, and the phosphorus content in filtrate is calculated in filtrate not
The carbon containing percentage composition of the theoretic molecule of sulfonation tannin that the quality of adsorbed additive for drilling fluid and manufacturer provide, root
According to following prediction equation, the absorption on clay after thinner sulfonation tannin is adsorbed 1.0 hours at a temperature of 150 DEG C is obtained
Amount, the results are shown in Table 1.
In the step 5), for calculating adsorbance of the sulfonation tannin on the clay under the high temperature conditions in drilling fluid
Prediction equation is：
Wherein, KAdsorbanceThe high temperature adsorption amount of-sulfonation tannin on clay, mgg-1；
mClayThe quality of clay, g in-drilling well liquid suspensions；
mInorganic agentThe quality of sulfonation tannin, g in-drilling well liquid suspensions；
mFiltrateThe quality of-filtrate, g；
The weight/mass percentage composition of organic carbon, % in P-filtrate；
Theoretical Mass percentage composition of the L-organic carbon in sulfonation tannin molecule, %.
Embodiment 2
The measure of high temperature (150 DEG C) adsorbance of thinner tannin in the weight % of argillaceous 4.0 drilling fluid
Experimental procedure is same as Example 1, and difference is, replaces sulfonation tannin using tannin, measurement result is shown in Table
1。
Embodiment 3
High temperature (150 DEG C) adsorbance of thinner ferrochrome lignosulfonate in the weight % of argillaceous 4.0 drilling fluid
Measure
Experimental procedure is same as Example 1, and difference is, sulfonation tannin is replaced using ferrochrome lignosulfonate,
Measurement result is shown in Table 1.
The embodiment 1-3 of table 1 measurement result
Note：According to《GB/T16783.1-2006 industrial gas oil drilling fluid on-the-spot test part 1s：Water-based drilling
Liquid》In assay method measure drilling well liquid suspensions AV and YP.
It is bigger that measurement result according to table 1 can be seen that adsorbance of the thinner on clay, drilling fluid system
AV and YP are smaller, that is, show that viscosity reducing effect is better.Illustrate that adsorbance of the processing agent molecule on clay end face is bigger, then increase
The degree of double electrode layer repulsion and aquation film thickness is bigger, so be more advantageous to break and weaken between clay particle by end-face and
The grid structure that end-end is formed by connecting is more obvious so as to reduce the effect of drilling fluid viscosity and shear force.Above experimental result meets
The mechanism of action of thinner, indicate the accuracy and validity of the method for the present invention.
Embodiment 4
Polymer-type fluid loss additive acrylamide/2- acrylamide-2-methyl propane sulfonics (monomer mole ratio 1:1,160
Time of equilibrium adsorption at DEG C in the weight % of argillaceous 4.0 drilling fluid is 7.50 minutes) in the weight % of argillaceous 4.0 brill
The measure of high temperature (160 DEG C) adsorbance in well liquid
Specific experiment step is as follows：
1) by above-mentioned polymer-type fluid loss additive acrylamide/2- acrylamide-2-methyl propane sulfonics, clay and water press than
Example is sufficiently mixed, and is configured to the drilling well liquid suspensions that fluid loss additive concentration is 2.0 weight %, and wherein clay weight accounts for clay and water
The 4.0% of gross weight.
2) above-mentioned drilling well liquid suspensions are added in high pressure high temperature filter tester, are warming up to 160 DEG C, pressure is arranged to
3.5MPa。
3) after 40 minutes, the back-pressure valve on high pressure high temperature filter tester is opened, casts out filtrate obtained by spurt loss, collects stable filter
The filtrate of high pressure high temperature filter tester bottom filter membrane is passed through under the conditions of mistake, records filtrate quality.
4) ICP-OES is utilized, determines the content of element silicon in filtrate, measurement result shows that its value is zero；Utilize organic carbon
Analyzer, the content of carbon in filtrate is determined, and brill not to be adsorbed in filtrate is calculated in the phosphorus content in filtrate
The quality of well liquid organic agent, and the theoretic molecule of the fluid loss additive is calculated according to the monomer mole ratio for forming molecule and contained
Carbon percentage composition, according to following prediction equation, obtain after the fluid loss additive is adsorbed 40 minutes at a temperature of 160 DEG C on clay
Adsorbance.
In the step 4), for calculating the used inorganic agent suction on the clay in drilling fluid under the high temperature conditions
The prediction equation of attached amount is：
Wherein, KAdsorbanceThe high temperature adsorption amount of-fluid loss additive on clay, mgg-1；
mClayThe quality of clay, g in-drilling well liquid suspensions；
mInorganic agentThe quality of fluid loss additive, g in-drilling well liquid suspensions；
mFiltrateThe quality of-filtrate, g；
The weight/mass percentage composition of organic carbon, % in P- filtrates；
Theoretical Mass percentage composition of the L- organic carbons in fluid loss additive molecule, %.
It the results are shown in Table 2.
Embodiment 5
Except carrying out carbon element content measure without using organic carbon analyzer, but organic blood urea/nitrogen analyzer is used instead to determine nitrogen
Constituent content, and substituted in the calculation with the content of organic nitrogen outside the content of organic carbon, other experimental procedures and embodiment 4
It is identical.It the results are shown in Table 2.
Embodiment 6
Polymer-type fluid loss additive acrylamide/2- acrylamide-2-methyl propane sulfonics/2- hydroxy-3-methyl acryloyls
Epoxide hydroxypropyltrimonium chloride (monomer mole ratio 4:5:Suction at 1,160 DEG C in the weight % of argillaceous 4.0 drilling fluid
Attached equilibration time is 6.0 minutes) measure of high temperature (160 DEG C) adsorbance in the weight % of argillaceous 4.0 drilling fluid
Except the fluid loss additive used replaces with acrylamide/2- acrylamide-2-methyl propane sulfonics/2- hydroxyl -3- first
Base acryloxypropyl trimethyl ammonium chloride (monomer mole ratio 4:5:1) outside, other experimental procedures and the phase of embodiment 4
Together.
Adsorbance of the fluid loss additive for measuring and being calculated under the high temperature conditions in drilling fluid on clay is shown in Table 2.
Embodiment 7
Except carrying out carbon element content measure without using organic carbon analyzer, but organic blood urea/nitrogen analyzer is used instead to determine nitrogen
Constituent content, and substituted in the calculation with the content of organic nitrogen outside the content of organic carbon, other experimental procedures and embodiment 6
It is identical.It the results are shown in Table 2.
Comparative example 1
There is provided with reference to high of heap of stone loss method (synthesis of heat-resistant salt-resistant fluid loss additive and the repercussion study with montmorillonite,
Shandong University's master thesis, 2010) it is measured.
1) by above-mentioned polymer-type fluid loss additive acrylamide/2- acrylamide-2-methyl propane sulfonics, clay and water press than
Example is sufficiently mixed, and is configured to the drilling well liquid suspensions that fluid loss additive concentration is 2.0 weight %, and wherein clay weight accounts for clay and water
The 4.0% of gross weight.
2) step 1) is prepared to obtained drilling well liquid suspensions and is placed in 25 DEG C of vibration 24h of constant temperature in oscillator, makes filtrate reducing
Agent is adsorbed in clay particle surface reaches balance.
3) the drilling well liquid suspensions for obtaining step 2) carry out magnetic agitation 24h, are placed in high temp roller furnace in 160 DEG C
Heat rolling aging 40 minutes.
4) it is quenched through cold water, is centrifuged 10 minutes under 10000 revs/min, take supernatant, and be diluted to 0~100mgL-1
In the range of, obtain testing sample.
5) TOC-4100 type organic carbon measuring instruments are utilized, organic carbon content in testing sample is determined, utilizes below equation meter
Calculate adsorbance.
Γ=(C0-C×A)/m
In formula, Г-adsorbance, mgg-1；
C0- inorganic agent initial concentration, mgL-1；
C- supernatants dilute post-treatment agent concentration, mgL-1；
A- extension rates；
Clay concentration in m- dispersions, gL-1。
Comparative example 2
Polymer-type fluid loss additive acrylamide/2- acrylamide-2-methyl propane sulfonics/2- hydroxy-3-methyl acryloyls
Epoxide hydroxypropyltrimonium chloride (monomer mole ratio 4:5:1) absorption in the weight % of argillaceous 4.0 drilling fluid measures
It is fixed
Experimental procedure is similar to comparative example 1, and difference is, uses acrylamide/2- acrylamide -2- methyl-prop sulphurs
Acid/2- hydroxy-3-methyl acryloxypropyls trimethyl ammonium chloride replaces acrylamide/2- acrylamide -2- methyl-prop sulphurs
Acid, measurement result are shown in Table 2.
The high temperature adsorption amount and high temperature and high pre ssure filtration of the two kinds of polymer type filtrate reducer for drilling fluid of table 2
Note：Normal temperature adsorbance be according to Yan Jie provide AAS (spectrophotometry SMP is on soil is removed
Adsorbance, Southwest Petroleum Institute journal, phase nineteen eighty-two the 1st) it is measured.The measurement temperature of filter pressing loss is 20 DEG C in normal temperature,
Pressure is 0.7MPa；The measurement temperature of high temperature and high pre ssure filtration is 160 DEG C, pressure 3.5MPa.
Measurement result according to table 2 can be seen that the different polymer-type fluid loss additive of two kinds of molecular structures normal
Adsorbance under the conditions of temperature is close, so as to which the influence of filter pressing loss in the normal temperature to the drilling fluid using its preparation is smaller.From height
The measurement result of warm adsorbance is understood, the data obtained using assay method of the present invention, is either used as spy using organic carbon
Sign element still usually determines using organic nitrogen as characteristic element, and the adsorbance result that it is measured is identical, is surveyed so as to be mutually authenticated
The reliability of test result.For mutually isostructural fluid loss additive, using the high temperature adsorption amount that method measure is lost value apparently higher than
The data obtained using assay method of the present invention, are illustrated in temperature-fall period, the fluid loss additive molecule in solution is gradually inhaled
It is attached on clay.In addition, the measure knot of the fluid loss additive high temperature adsorption amount of two kinds of different molecular structures is determined using the method that is lost
Fruit is close, it is impossible to the difference of the high temperature and high pre ssure filtration of corresponding drilling fluid is reasonably explained, so as to handling agent molecule
Improved reference value effect is smaller.It in summary it can be seen, under hot conditions, 2- hydroxy-3-methyls acryloxypropyl three
Ammonio methacrylate is favorably improved adsorbance of the fluid loss additive molecule on clay as strong suction-operated monomer, so as to contribute to
Improve the filtration property of drilling fluid.This has also further demonstrated that the size of drilling fluid organic process agent molecule adsorbance on clay
The performance of inorganic agent under the high temperature conditions is directly influenced to play, what the result measured using assay method of the present invention was reflected
It is actual adsorbance of the inorganic agent on clay under hot conditions, can is to research and develop new temperature resistance inorganic agent, optimize at temperature resistance
Reason agent molecule structure provides strong technical support.
Claims (5)
1. a kind of assay method of drilling fluid organic agent absorption property, comprises the following steps：
A) the drilling fluid organic agent, clay and water are mixed, obtains drilling well liquid suspensions；
B) the drilling well liquid suspensions are subjected to heat filtering；
C) content of the carbon and/or nitrogen in filtrate is determined；
Wherein, methods described is additionally included in the step c-1 before step c))：Determine the content of the element silicon in filtrate；
The step b) comprises the following steps：
B1) the drilling well liquid suspensions are added in high pressure high temperature filter tester, are warming up to predetermined temperature；
B2) after reaction to the scheduled time, the filtrate that filter membrane is passed through in high pressure high temperature filter tester is collected；
The step c-1) include when the silicon content in filtrate is not zero, it is the smaller filter in aperture by the filter membrane replacing
Film and repeat step a)~c-1), until the silicon content in filtrate is zero；
Methods described is also including drilling fluid not to be adsorbed in the carbon in filtrate or the cubage filtrate of nitrogen
The quality of organic agent, and then calculate and obtain adsorbance of the drilling fluid organic agent on clay；
Adsorbance of the drilling fluid organic agent on clay is calculated by Formulas I：
Wherein, KAdsorbanceAdsorbance of-drilling fluid the organic agent on clay, mgg-1；
mClayThe quality of clay in-drilling well liquid suspensions, g；
mInorganic agentThe quality of drilling fluid organic agent in-drilling well liquid suspensions, g；
mFiltrateThe quality of-filtrate, g；
The weight/mass percentage composition of carbon or nitrogen in P- filtrates, %；
The Theoretical Mass percentage composition of L- carbons or nitrogen in drilling fluid organic process agent molecule, %.
2. according to the method for claim 1, it is characterised in that the drilling fluid organic agent is selected from thinner, drop filter
Lose the one or more in agent, coating agent, tackifier, flocculant, surfactant and inhibitor.
3. method according to claim 1 or 2, it is characterised in that the predetermined temperature is 85-260 DEG C.
4. according to the method for claim 3, it is characterised in that the predetermined temperature is 100-220 DEG C.
5. according to the method for claim 1, it is characterised in that carbon is measured using organic carbon analyzer, adopted
Nitrogen is measured with organic blood urea/nitrogen analyzer.
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| CN102174314A (en) * | 2011-03-09 | 2011-09-07 | 西南石油大学 | Organic silicon fluid loss additive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102174314A (en) * | 2011-03-09 | 2011-09-07 | 西南石油大学 | Organic silicon fluid loss additive and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 抗高温有机硅共聚物降滤失剂的合成与性能;褚奇 等;《石油化工》;20111231;第40卷(第9期);991-996 * |
| 耐温抗盐聚合物钻井液降滤失剂的合成与评价;朱腾;《中国优秀硕士学位论文全文数据库（电子期刊），工程科技Ⅰ辑》;20130215;B019-7 * |
| 钻井液处理剂在重晶石表面吸附行为研究;王平全 等;《钻井液与完井液》;20140131;第31卷(第1期);8-11 * |
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