CN105567181A - Production method of novel organic rectorite for oil-based drilling fluid - Google Patents
Production method of novel organic rectorite for oil-based drilling fluid Download PDFInfo
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- CN105567181A CN105567181A CN201510893277.6A CN201510893277A CN105567181A CN 105567181 A CN105567181 A CN 105567181A CN 201510893277 A CN201510893277 A CN 201510893277A CN 105567181 A CN105567181 A CN 105567181A
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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
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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
- C09K8/32—Non-aqueous well-drilling compositions, e.g. oil-based
Abstract
Disclosed is a production method of novel organic rectorite for oil-based drilling fluid. The organic rectorite comprises rectorite and quaternary ammonium salt as main components. The production method includes the steps of A, sodium-modification/lithiation pretreatment; B, organic modification reaction; C, filtering and washing; and D, ageing, drying and grinding. The production method has the advantages that since calcium-based rectorite raw material is subjected to the sodium-modification/lithiation pretreatment according to the sodium salt and lithium salt compound modification technology, colloid rheological property of the organic rectorite product is improved; chemical reaction of organic-modification cation exchange is promoted completely by a controllable high-temperature organic modification process, and thus quality of the organic rectorite is much stable; residual dissoluble ion of products from the organic modification cation exchange reaction is removed by a washing and filtering process, so that high-temperature stability of the products is improved further while content of impurity thereof is reduced.
Description
Technical field
The present invention relates to the production technology of the industries such as a kind of oil, Sweet natural gas, Di Kuang, construction work for the colloidal materials of drilling fluid, belong to drilling well compositions field.Relate in particular to a kind of production method of organic clay for oil base drilling fluid.
Background technology
Oil base drilling fluid has high temperature resistance, anti-salt, stabilizing borehole, be beneficial to lubrication and to advantages such as formation damage degree are less, be international mainstream drilling fluid, external most of drilling engineering have employed oil base drilling fluid.The domestic advantage also recognizing oil base drilling fluid, in conjunction with the stratum condition of drilling well project, just progressively improves the usage ratio of oil base drilling fluid.
Organic clay is the indispensable oleophylic colloid material of oil base drilling fluid.Rectorite leng is as a kind of novel clay soil that can be used for drilling fluid, and in rheological, high-temperature stability, filtration reduction etc., have original feature, be the potential upgraded product of drilling fluid field tool.Patent 01133501.7, patent 201010262766.9 indicate these advantages of rectorite leng, but they relate to is sodium base rectorite leng for water base drilling fluid system.To for oil base drilling fluid, rectorite leng has to pass through organically-modified, makes organic rectorite.Patent 201010258856.0 discloses a kind of oil base drilling fluid organic rectorite and production method thereof, calcium base rectorite leng is characterized in mix with the quaternary ammonium salt solution as organic insulating covering agent, the method of shear extrusion is adopted to organise, the fricative heat of cal rolling is utilized to realize organising, and then drying is finished product with pulverizing, it is a kind of simply low cost working method.
Although the technology disclosed in patent 201010258856.0 has the advantages such as technique is simple, easy to operate, with low cost, also there are some problems.
The first, the technology disclosed in patent 201010258856.0 is directly raw material with calcium base rectorite leng, affects the effect organised.Industrial, clay, generally will through sodium modification or activation modification before organising.The know-why of sodium modification is, sodium ion is monovalent ion, and after sufficient cationic exchange, ion concentration divalent calcium ions doubles, Na
+, Ca
++electro kinetic potential is suitable, therefore the total electro kinetic potential of Na type clay is approximately the twice of Ca type clay, and the polar molecule that Na type clay particle adsorbs is more, adsorption film is thicker, the charge repulsion that the micelle formed produces each other is larger, and micelle particulate not easily assembles sedimentation, and soliquid is more stable.The quality of the colloidal property of the finished product organophilic clay of sodium/organise and alkali metal ion content measured positive correlation, with total electro kinetic potential positive correlation, a large amount of simultaneous test confirms this point.Non-natural sodium form clay mineral can obtain through sodium modification the effect that organises preferably.Li and Na is all alkali metal, Li
+electro kinetic potential compares Na
+higher, the colloidal property of Li type clay is better.But independent lithiumation pre-treatment or the pretreated organophilic clay production method of sodium/lithiumation compound, there is not yet open report.The know-why of activation modification is, the adsorptive power of clay mineral is proportional to specific surface area, after mineral acid activation, specific surface area increases, be conducive to realizing organic cations to exchange and absorption, be conducive in dispersion system, form thicker, more stable micelle particulate, and can stripping part Al in acidization
+++, Mg
++ion, adds the exchangeable cationic type between layer amount.Industrial production organobentonite is nothing more than carrying out sodium, acid activation two kinds of pre-treatment, and its core technology principle as above.So, in order to make rectorite leng raw material better participate in the cation exchange reaction that organises, sodium (or lithiumation) or activation modification process need be carried out to rectorite leng.
The second, the technology disclosed in patent 201010258856.0 does not heat in the process of organising, and only maintain cation exchange reaction by rolling fricative heat, organise less effective.Test shows, only by frictional heat, temperature of charge only can maintain 30 ~ 60 DEG C usually, and summer can reach 70 ~ 80 DEG C once in a while.Be thermo-negative reaction with the chemical reaction that quaternary ammonium salt carries out cationic exchange as organic insulating covering agent to rectorite leng, improve temperature of reaction and be conducive to chemical equilibrium and carry out towards the direction generating organic rectorite, therefore the low effect that must affect the reaction that organises of temperature.On the other hand, according to the technology disclosed in patent 201010258856.0, temperature of charge is greatly influenced by ambient temperature, and seasonal fluctuation is large, and difficult quality controls.So, in order to organifying sufficient reacting carries out, need higher, more controlled temperature of reaction.
3rd, the technology disclosed in patent 201010258856.0 is left to organise the Ca of reacting final product
++ion, Mg
++ion, Cl
-the impurity such as ion retain in the product, do not wash, affect product performance to end product.The disadvantageous effect of these ion pair products is divided into two aspects.On the one hand, due to the effect of these hetero-ions, the high-temperature stability of oil systems is deteriorated, and after high temperature ageing, the viscosity of drilling fluid system is easy to multiviscosisty, and drilling rod moment of torsion increases, but also causes filter loss to increase.On the other hand, remaining hetero-ion is impurity, causes the effective content of organophilic clay to reduce, and in order to obtain same effect, just has to improve as the add-on of oleophylic colloid in all oil system or water-in-oil system.So, in order to ensure the performance of product, should wash to remove foreign ion to end product after the reaction that organises.Organoclay is divided into wet method and dry method, and the major reason that wet method is better than dry method is just that being convenient to washing removes foreign ion.
Summary of the invention
For the deficiency of published organic rectorite production method, the object of the present invention is to provide a kind of production method of improvement, the oil base drilling fluid organic rectorite product that, performance higher with the quality of production is more stable.
Production stage of the present invention is:
(1) sodium/lithiumation pre-treatment.In the container filling 75 ~ 90 parts of calcium base rectorite leng raw materials, add the mixture of 2 ~ 10 parts of sodium salts and lithium salts and 1 ~ 20 times to the process water of calcium base rectorite leng raw material, be warming up to 70 ~ 95 DEG C.Stirring at low speed 30 ~ 210 minutes, forms uniform slurries.
(2) organise reaction.Organic for quaternary ammonium salt insulating covering agent 10 ~ 25 parts is joined in above-mentioned slurries, heats while stirring, temperature is controlled at 70 ~ 115 DEG C.If the temperature of reaction of setting is greater than 100 DEG C, this container is then necessarily airtight, is greater than an atmospheric pressure to obtain in container, ensures that slurries are unlikely to gasification.After reaching design temperature, be incubated 30 ~ 210 minutes while stirring.
(3) filter, wash.
(4) ageing, drying, pulverizing.
Described calcium base rectorite leng raw material is natural accumulation supporting stone raw ore or the rectorite leng concentrate after sorting, rectorite leng content >=55%, and the calcium ion type accounting in rectorite leng interlayer cation reaches more than 50%.
Pretreatment technology is one of innovative point of the present invention.Composite modified with sodium salt/lithium salts, sodium salt is that one or both of sodium carbonate or sodium-chlor mix with arbitrary proportion, and lithium salts is that Quilonum Retard, lithium chloride or lithium oxalate wherein one or more mix with arbitrary proportion.Sodium salt: the ratio of mixture of lithium salts is 1:99 ~ 99:1.We adopt the composite modified technique of sodium/lithiumation first in the production of organophilic clay.In 25 DEG C of acidic solutions, [Li
+]+[e-] standard potential of=[Li] reaction formula is-3.0401v, is the electropotential that in all elements, absolute value is the highest.Li and Na is all alkali metal, Li
+electro kinetic potential compares Na
+higher, therefore, the colloidal property of Li type clay is better, and specifically, directly organise relative to calcium base rectorite leng and organise after sodium modification, after sodium/lithiumation is composite modified, organophilic clay product can obtain better rheological property in oil-base mud.And after lithiumation process and follow-up organic-treating, it is clean that a small amount of interlayer lithium ion that the interlayer of organic rectorite still adsorbs is that filtration washing is difficult to remove, and this part lithium ion is useful for the high-temperature stability improving organophilic clay.Consider that the normal-temperature dissolution degree of several lithium salts in water is not high, we need to keep higher temperature when sodium/lithiumation process, the effect of strengthening sodium/lithiumation modification.
Described sodium salt is one or both mixtures mixed with arbitrary proportion of sodium carbonate or sodium-chlor, lithium salts is Quilonum Retard, lithium chloride or lithium oxalate one or more mixtures mixed with arbitrary proportion wherein, sodium salt: the ratio of mixture of lithium salts is 1:99 ~ 99:1.
The organic insulating covering agent of described quaternary ammonium salt be m-alkylpolyoxyethylene or/and n-alkyl-dimethyl benzyl ammonium halide, m, n are the carbonatoms of carbochain, and its value is 10 ~ 24.
Organise reaction time, temperature of reaction is at least higher than the fusing point of used quaternary ammonium salt.Heating is conducive to quaternary ammonium salt and dissolves, ionizes, and improves the momentum of molecular motion, can fully react.
Described filtration and washing are that the product slurry of the reaction that organises is moved into the devices such as common plate-and-frame filter press, diaphragm filter press, vacuum filtration machine or whizzer, elimination moisture and soluble ion as far as possible.Repeatedly repeatedly should dilute filter wash if desired.The number of times of filter wash supplements the difference of the accumulative thinning ratio added water and different depending on the amount of process water that adds during sodium/lithiumation pre-treatment and filter wash, and requirement is that the content of the remaining soluble ion ensureing product is lower than 1% of parent ion content.In general, the final replaced organic cation of coming in of product is The more the better, and its limit is exactly the cation exchange capacity of mineral.Within the scope of saturated add-on, organic insulating covering agent add-on is more, and performance is better.Exceeding saturated add-on nonsensical, can be rinsed when washing.
Described ageing be by press filtration wash after filter cake or the In Shade stacking of similar dewatered product more than 8 hours.
Described drying be by ageing after product under 100 ~ 150 DEG C of environment, be dried to water ratio be less than 3.5%.
Described pulverizing adopts pulverizer dried product to be ground into 80 orders or thinner (median size is less than or equal to 0.173mm).
Organic rectorite of the present invention compares with organobentonite, still has larger cost advantage, because organic insulating covering agent add-on can be less than organobentonite greatly.We know, the cation exchange capacity (CEC) of rectorite leng is 36 ~ 40mmol/100g, and wilkinite CEC is generally 70 ~ 100mmol/100g, and rectorite leng only needs less organic insulating covering agent just can to reach capacity cation exchange capacity.
Although the present invention is relative to original patent 201010258856.0, suitably cost can be increased in technologic improvement, but for organobentonite, Material Cost of the present invention is low, comprehensive cost still has very high competitive power, performance then all improves a lot than the technology of original similar rectorite leng and bentonitic technology, and therefore, the present invention brings the stronger market competitiveness to product.
Embodiment
Embodiment 1.
In reaction vessel, add the calcium base rectorite leng powder (100 order) that 100 parts of purity are 66% water ratio 6%, add the mixing solutions of 2 parts of sodium carbonate, 1.5 parts of Quilonum Retards, 200 parts of water, then add 200 parts of process waters, heating is also stirred with the speed of 120rpm, temperature is risen to 90 DEG C.Keep stirring 45 minutes, get the palmityl trimethyl ammonium chloride 20 parts of net content 75% (all the other are mainly water), add container, vessel temp is remained on 90 DEG C, continue to stir with the speed of 120rpm, organise reaction 90 minutes.Add 200 parts of room temperature process waters, stir 2 minutes, to adjust the thinning ratio of slurries.Subsequently, slurries are imported vacuum filtration machine and carry out suction filtration, take out filter cake, in cool place place placement 24 hours, dry to water content 3%.Be crushed to 200 orders (0.074mm), the organic rectorite of obtained embodiment 1.Record performance perameter in table 1.
Comparative example 1.
It is the calcium base rectorite leng powder (100 order) of 66% water ratio 6% by 100 parts of purity, be placed in industrial sand mill, organic insulating covering agent palmityl trimethyl ammonium chloride of 75% net contents of 20 parts (all the other are water) is heated to 30 DEG C, add the process water of 5 parts 70 DEG C, organic insulating covering agent is made to have mobility, again this organic insulating covering agent is added to sand mill, adjustment muller gap makes reactive force larger, shear extrusion is implemented to mixture, the time of shear extrusion is 90 minutes, material is released from sand mill, ageing places 24 hours, oven dry to water content is 6%, levigate to particle diameter 200 order (0.074mm) with Raymond machine, the organic rectorite of obtained comparative example 1.Record performance perameter in table 1.
Embodiment 2.
In sealable reaction vessel, add the calcium base rectorite leng powder that 100 parts of purity are 73% water ratio 6.5%, add the mixing solutions of 3 parts of sodium carbonate, 2 parts of lithium oxalates, 200 parts of water, then add 300 parts of process waters, heating is also stirred with the speed of 120rpm, temperature is risen to 80 DEG C.Keep stirring 45 minutes, get the stearyl dimethyl benzyl ammonium chloride 28.5 parts of net content 75% (all the other are mainly water), add container, vessel temp is remained on 115 DEG C and in encloses container build-up pressure, continue to stir with the speed of 120rpm, be incubated 60 minutes.Subsequently, slurries are imported vacuum filtration machine and carry out suction filtration, when filtrate discharge goes out about 80%, when the concentration of remaining slurry obviously increases in suction funnel, add process water 400 parts again, suction filtration again, drains moisture, take out filter cake, place 48 hours, dry to water ratio 3%.Be crushed to 200 orders (0.074mm), the obtained organic rectorite to embodiment 2.Record performance perameter in table 1.
Comparative example 2.
It is the calcium base rectorite leng powder (100 order) of 73% water ratio 6.5% by 100 parts of purity, be placed in industrial sand mill, organic insulating covering agent stearyl dimethyl benzyl ammonium chloride of 75% net contents of 28.5 parts (all the other are water) is heated to 30 DEG C, add the process water that 5 parts of temperature are 70 DEG C, organic insulating covering agent is made to have mobility, again this organic insulating covering agent is added to sand mill, adjustment muller gap makes reactive force larger, shear extrusion is implemented to mixture, the time of shear extrusion is 60 minutes, material is released from sand mill, ageing places 48 hours, oven dry to water content is 6%, levigate to particle diameter 200 order (0.074mm) with Raymond machine, the organic rectorite of obtained comparative example 2.Record performance perameter in table 1.
The performance test results of table 1 embodiment and comparative example
Note: high temperature rheology and high temperature fluid loss performance system sample heat at 180 DEG C rolls 16h and the performance measured after being cooled to room temperature 25 DEG C.
Testing method explanation
Colloidity: accurately take 4.0g organic rectorite (being accurate to 0.01g), pours into and fills in No. 0 clean diesel mud cup of 200ml, mud cup height 18cm, upper end diameter 9.7cm, lower end diameter 7.0cm.Under 4000rpm, stir 2min with homogenizer, make it disperse completely.Homogenizer blade diameter 2.5cm, quality 5.5g.Therefrom measuring 100ml mixed solution pours in the tool plug graduated cylinder of 100ml, after jam-pack graduated cylinder, hand 5 minutes up and down, leaves standstill 90 minutes, observes and records upper strata and to dissociate the volume V (ml) of diesel oil.The formula calculating colloidity is as follows:
Colloidity=(100-V)/l00 × 100%.
The measuring method of rheological property: these rheological property indexs of apparent viscosity, plastic viscosity, yield value can pass through viscosimetric analysis.Accurately take 10.5g organic rectorite (being accurate to 0.01g), pour in the mud cup of No. 0 clean diesel filling 350ml, under 4000rpm, stir 2min with homogenizer, take off mud cup, scrape the rectorite leng sticking to container side wall, bottom surface.Then, high-speed stirring 10min under 11000rpm rotating speed.Measure Φ 600, Φ 300 by direct-reading type at normal temperatures and read value, instrument is FANN35 type.Calculate apparent viscosity, plastic viscosity, yield value according to the following formula.
Apparent viscosity AV=1/2 [Φ 600 reads value], (mPas)
Plastic viscosity PV=[Φ 600 reads value]-[Φ 300 reads value], (mPas)
Yield value YP=AV-PV, (Pa)
The measuring method of filter loss: under 25 DEG C of room temperatures, accurately measure No. 0 clean diesel of 380ml, pour in mud cup, add 20ml distilled water, add 12.0g organic rectorite, under 4000rpm, stir 2min with homogenizer, take off mud cup, scrape the rectorite leng sticking to container side wall, bottom surface.Then, high-speed stirring 10min under 11000rpm rotating speed, takes off.Poured into by above-mentioned suspension in the mud box of drying of filtration device immediately, make liquid level to top be about 13mm place, add sealing-ring and filter paper and after capping, Quick-pressing is to 0.69MPa, and during record 30min, the milliliter number of the volume of filtrate in graduated cylinder, is filter loss.
High temperature rheology, high temperature filter loss measure: under 11000rpm rotating speed after high-speed stirring, sample loads stainless cylinder of steel, is filled with 1.0MPa nitrogen, and 180 DEG C of heat roll 16h, take out, are cooled to 25 DEG C of room temperatures, as stated above flow measurement sex change and filter loss.
Claims (8)
1. a production method for oil base drilling fluid organic rectorite, is characterized in that comprising the following steps:
(1) sodium/lithiumation pre-treatment: add the mixture of 2 ~ 10 parts of sodium salts and lithium salts and 1 ~ 20 times to the process water of calcium base rectorite leng raw material in the container filling 75 ~ 90 parts of calcium base rectorite leng raw materials, be warming up to 70 ~ 95 DEG C, stirring at low speed 30 ~ 210 minutes, forms uniform slurries;
(2) organise reaction;
Organic for quaternary ammonium salt insulating covering agent 10 ~ 25 parts is joined in above-mentioned slurries, heat while stirring, temperature is controlled at 70 ~ 115 DEG C, if the temperature of reaction of setting is greater than 100 DEG C, this container is then necessarily airtight, to obtain in container and to be greater than an atmospheric pressure, ensure that slurries are unlikely to gasification;
After reaching design temperature, be incubated 30 ~ 210 minutes while stirring;
(3) filter, wash;
(4) ageing, drying, pulverizing.
2. the production method of a kind of oil base drilling fluid organic rectorite according to claim 1, it is characterized in that calcium base rectorite leng raw material is natural accumulation supporting stone raw ore or the rectorite leng concentrate after sorting, rectorite leng content >=55%, the calcium ion type accounting in rectorite leng interlayer cation reaches more than 50%.
3. the production method of a kind of oil base drilling fluid organic rectorite according to claim 1, it is characterized in that sodium salt is one or both mixtures mixed with arbitrary proportion of sodium carbonate or sodium-chlor, lithium salts is Quilonum Retard, lithium chloride or lithium oxalate one or more mixtures mixed with arbitrary proportion wherein, sodium salt: the ratio of mixture of lithium salts is 1:99 ~ 99:1.
4. the production method of a kind of oil base drilling fluid organic rectorite according to claim 1, it is characterized in that the organic insulating covering agent of quaternary ammonium salt is that m-alkylpolyoxyethylene is or/and n-alkyl-dimethyl benzyl ammonium halide, m, n are the carbonatoms of carbochain, and its value is 10 ~ 24.
5. the production method of a kind of oil base drilling fluid organic rectorite according to claim 1, it is characterized in that filtration and washing are that the product slurry of the reaction that organises of step (2) is moved into common plate-and-frame filter press, diaphragm filter press, vacuum filtration machine or whizzer, elimination moisture and soluble ion, repeatedly repeatedly should dilute filter wash if desired, the amount of the process water that the number of times of filter wash adds depending on step (1) and filter wash supplement the difference of the accumulative thinning ratio added water and different, requirement is that the content of the remaining soluble ion ensureing product is lower than 1% of parent ion content.
6. the production method of a kind of oil base drilling fluid organic rectorite according to claim 1, it is characterized in that ageing be by press filtration wash after filter cake or the In Shade stacking of similar dewatered product more than 8 hours.
7. the production method of a kind of oil base drilling fluid organic rectorite according to claim 1, it is characterized in that drying be by ageing after product under 100 ~ 150 DEG C of environment, be dried to water ratio be less than 3.5%.
8. the production method of a kind of oil base drilling fluid organic rectorite according to claim 1, is characterized in that pulverizing is that dried product is ground into 80 orders by employing pulverizer or median size is less than or equal to 0.173mm.
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| CN106634882A (en) * | 2016-09-19 | 2017-05-10 | 武汉华矿胶体化学有限公司 | Organic rectorite composition for oil-based drilling fluid and preparation method of organic rectorite composition |
| CN114539992A (en) * | 2022-03-01 | 2022-05-27 | 武汉华矿胶体化学有限公司 | Improved organic rectorite for oil-based drilling fluid and preparation method thereof |
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| CN101942292A (en) * | 2010-08-23 | 2011-01-12 | 湖北美标汽车制冷系统有限公司 | Organic clay for oil base drilling fluid and production process thereof |
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| CN101942292A (en) * | 2010-08-23 | 2011-01-12 | 湖北美标汽车制冷系统有限公司 | Organic clay for oil base drilling fluid and production process thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106634882A (en) * | 2016-09-19 | 2017-05-10 | 武汉华矿胶体化学有限公司 | Organic rectorite composition for oil-based drilling fluid and preparation method of organic rectorite composition |
| CN114539992A (en) * | 2022-03-01 | 2022-05-27 | 武汉华矿胶体化学有限公司 | Improved organic rectorite for oil-based drilling fluid and preparation method thereof |
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