CN115626963A - Oil-based drilling fluid centrifugate flocculant, preparation method thereof and application thereof in flocculation recovery of oily drilling cutting centrifugate - Google Patents
Oil-based drilling fluid centrifugate flocculant, preparation method thereof and application thereof in flocculation recovery of oily drilling cutting centrifugate Download PDFInfo
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Abstract
The invention provides an oil-based drilling fluid centrifugate flocculating agent, a preparation method thereof and application thereof in flocculating recovery of an oil-containing drilling cutting centrifugate. The preparation method of the oil-based drilling fluid centrifugate flocculant comprises the following steps: adding pretreated styrene, 4-vinylpyridine and a cationic monomer into a solvent, stirring to disperse the mixture uniformly, and then heating to a reaction temperature; then adding an initiator to carry out constant temperature reaction; and after the reaction is finished, cooling to room temperature, adding methanol into the obtained reaction liquid to separate out a polymer, and then filtering and drying to obtain the oil-based drilling fluid centrifugal liquid flocculant. The flocculant provided by the invention adopts the oil-soluble monomer as a main raw material, so that the flocculant can be ensured to have good solubility in the oil-based drilling fluid, and can flocculate the micro-scale poor solid phase in the centrifugate of the oil-based drilling fluid. The centrifugate flocculated by the flocculating agent can be reused for preparing the oil-based drilling fluid, so that the utilization rate of the centrifugate of the oil-based drilling fluid is improved.
Description
Technical Field
The invention relates to an oil-based drilling fluid centrifugate flocculant, a preparation method thereof and application thereof in flocculation recovery of an oil-containing drilling cutting centrifugate, belonging to the field of oilfield chemistry of the petroleum industry.
Background
Along with the large-scale development of unconventional oil and gas resources such as shale oil and gas, the drilling number of complex wells such as deep wells, ultra-deep wells, horizontal wells and the like is gradually increased. The oil-based drilling fluid is widely applied to unconventional oil and gas development due to good temperature resistance, lubricity, inhibitive performance and the like.
The oil-based drilling fluid has limited rock carrying capacity in the drilling process of the horizontal well, a large amount of rock debris is repeatedly and circularly ground in the well, the particle size is greatly reduced, and the tertiary solid control equipment is difficult to remove, so that the inferior solid phase content in the drilling fluid is high finally.
The oil-based drilling fluid can generate a large amount of oily drill cuttings in the drilling process, and the oily drill cuttings are dangerous waste and high in treatment cost. The field usually uses a three-stage solid control device represented by a vibrating screen, a drier and a centrifuge to carry out deoiling treatment on the oily drilling cuttings. In the process, the rock debris treated by the vibrating screen still contains a large amount of oil-based drilling fluid, in order to reduce the rock debris, a drier is used for drying the part of the rock debris on site, the liquid discharged after drying enters a high-speed centrifuge for further treatment, and the solid phase generated in the drying and centrifuging processes is transported to a specialized factory for separate treatment. If the density of the oil-based drilling fluid is low and the viscosity of the centrifugate generated after high-speed centrifugation is low, the part of the centrifugate can be re-prepared for use; if the density of the oil-based drilling fluid is high, the treated centrifugate has high content of low-density inferior solid phase, high viscosity, difficult reutilization and high treatment cost. Through statistics, 40-60 square of centrifugate is generated in the drilling process of the single-hole oil-based drilling fluid in Chongqing areas, and the part of centrifugate cannot be repeatedly prepared due to overhigh content of inferior solid phase. If the oily drilling cutting centrifugate is not properly treated, resources are wasted, and serious environmental pollution can be caused.
The flocculation technology is one of effective means for solving the problems that the particle size of the harmful solid phase is too small and the harmful solid phase is difficult to remove from the centrifugate. However, most of the existing flocculation technologies are directed at water-soluble flocculants of water phases, and cannot play a role in a nonpolar dispersion system of oil-based drilling fluid centrifugate mainly comprising an oil phase. Chinese patent document CN114605582A provides an oil-based drilling fluid flocculant, which comprises the following raw materials in parts by weight: 14 to 20 portions of emulsifier, 90 to 110 portions of styrene, 30 to 40 portions of methacrylate, 10 to 20 portions of fatty acid, 6 to 12 portions of p-hydroxystyrene, 0.8 to 1.6 portions of oil-soluble initiator and 90 to 100 portions of deionized water. Chinese patent document CN113292731A provides a flocculant for removing rock debris of oil-based drilling fluid, wherein the flocculant is prepared by performing graft polymerization reaction on prepolymer A and prepolymer B in the presence of a third solvent; wherein the prepolymer A is prepared by a first polymerization reaction of a hydrophilic monomer, a cationic monomer and glycidyl methacrylate in the presence of a first solvent and a first initiator; the prepolymer B is prepared by carrying out second polymerization reaction on oil-soluble monomers, acrylamide and 2-mercaptoethylamine hydrochloride in the presence of a dispersant, a second solvent and a second initiator. The flocculant has the characteristic of selectively flocculating rock debris in oil-based drilling fluid, and can effectively enhance the removal effect of fine rock debris under the cooperation of solid control equipment. Chinese patent document CN113773439A provides a flocculant for an oil-based drilling fluid, wherein the flocculant is modified cationic polyacrylamide, and raw materials for preparing the flocculant comprise the following components in parts by weight: 40-60 parts of acrylamide, 5-15 parts of quaternary ammonium salt cationic monomer, 1-5 parts of sodium acrylate, 0.05-0.15 part of initiator, 0.1-0.5 part of sodium ethylene diamine tetracetate, 0.05-0.1 part of urea, 5-15 parts of surfactant and 30-60 parts of solvent. However, the flocculant prepared by the patent is used for treating the solid phase in the oil-based drilling fluid, and the oil-based drilling fluid has larger solid phase particle size and smaller treatment difficulty; the poor solid phase in the oil-based drilling fluid centrifugate has small particle size and high treatment difficulty, and the flocculant is not suitable for use.
Therefore, a flocculant for the oil-based drilling fluid centrifugate needs to be developed to realize resource utilization of the oil-based drilling fluid oil-containing drilling cutting centrifugate and provide technical support for safe, rapid and efficient drilling.
Disclosure of Invention
The invention provides an oil-based drilling fluid centrifugate flocculant, a preparation method thereof and application thereof in flocculation recovery of an oil-containing drilling fluid centrifugate, aiming at the defects of the prior art, particularly the problems that the existing solid control equipment has limited cleaning capacity for low-density harmful solid phases and the prior art lacks a method for removing harmful solid phases in the oil-based drilling fluid oil-containing drilling fluid centrifugate.
The technical scheme adopted by the invention is as follows:
a preparation method of an oil-based drilling fluid centrifugate flocculant comprises the following steps:
adding pretreated styrene, 4-vinylpyridine and cationic monomer into a solvent, stirring to uniformly disperse the styrene, the 4-vinylpyridine and the cationic monomer, and then heating to a reaction temperature; then adding an initiator to carry out constant temperature reaction; and after the reaction is finished, cooling to room temperature, adding methanol into the obtained reaction liquid to separate out a polymer, and then filtering and drying to obtain the oil-based drilling fluid centrifugal liquid flocculant.
According to the present invention, preferably, the solvent is a mixed solution of ethanol and toluene, and the mass ratio of ethanol to toluene in the mixed solution is 1.
According to the invention, the styrene is preferably pretreated by: washing styrene for 3 times by using NaOH aqueous solution with the mass fraction of 10-20%; in each washing process, the mass ratio of the styrene to the NaOH aqueous solution is 1.
According to the invention, the cationic monomer is preferably one or the combination of more than two of dimethyldiallylammonium chloride, dodecyl methyl diallylammonium chloride and acryloyloxyethyl trimethyl ammonium chloride; the structural formula of the dodecyl methyl diallyl ammonium chloride is shown as a formula I.
It is preferred according to the present invention that the pretreated styrene is 6 to 16 parts, 4-vinylpyridine 12 to 18 parts, cationic monomer 18 to 26 parts, based on 100 parts by weight of the solvent; it is further preferable that the pretreated styrene is 8 to 14 parts, the 4-vinylpyridine is 14 to 16 parts, and the cationic monomer is 20 to 24 parts, based on 100 parts by weight of the solvent.
According to the invention, the initiator is preferably one of benzoyl peroxide, azobisisobutyronitrile and tert-butyl hydroperoxide; the mass of the initiator is 0.3-0.8% of the total mass of the pretreated styrene, 4-vinylpyridine and cationic monomer.
According to the present invention, the reaction temperature is preferably 60 to 80 ℃, more preferably 65 to 75 ℃.
According to the invention, the isothermal reaction time is preferably 10 to 20 hours, more preferably 12 to 18 hours.
According to the present invention, the volume ratio of methanol to the reaction solution is preferably 3 to 5.
According to the invention, the drying is preferably carried out at 50-70 ℃ for 10-15h under vacuum.
The invention also provides a flocculant of the oil-based drilling fluid centrifugate, which is prepared by the preparation method.
According to the invention, the application of the oil-based drilling fluid centrifugate flocculant in the flocculation recovery of the oil-based drilling fluid oily drilling cutting centrifugate comprises the following specific application methods: under the condition of stirring, adding the prepared oil-based drilling fluid centrifugate flocculant into the oil-containing drilling cuttings centrifugate of the oil-based drilling fluid, transferring the oil-based drilling fluid centrifugate flocculant into a centrifuge for centrifugation after uniform dispersion, and collecting the centrifuged centrifugate to realize recycling of the oil-containing drilling cuttings centrifugate; the stirring rotating speed is 500-3000rpm, the mass of the oil-based drilling fluid centrifugate flocculant is 0.1-5% of the mass of the oil-based drilling fluid oily drilling cutting centrifugate, and the centrifugation rotating speed is 1500-3500rpm.
The invention has the following technical characteristics and beneficial effects:
1. the flocculant provided by the invention adopts the oil-soluble monomer as a main raw material, so that the flocculant can be ensured to have good solubility in the oil-based drilling fluid.
2. The flocculant synthesized by the invention is a cationic polymer and can flocculate micro-scale poor solid phases in the oil-based drilling fluid centrifugate. The flocculant synthesized by the method contains a large amount of cations, has a large molecular weight, can be combined with a micro-scale inferior solid phase in the oil-based drilling fluid centrifugate through electrostatic interaction, increases the volume and the mass of the inferior solid phase, and is easier to separate from the centrifugate through a centrifugation method. The proportion of each monomer and the addition of the initiator in the preparation process of the flocculant are very important. Whether the monomer proportion is proper or not determines the quantity of cations in the flocculant, the cations are less and are unfavorable for the flocculation capacity of the flocculant, and meanwhile, the cation proportion cannot be too high, so that the flocculation performance of the flocculant is reduced; the addition of the initiator cannot be too large, so that the molecular weight of the initiator is reduced, the flocculation capacity of the flocculant is reduced due to low molecular weight, and the flocculation capacity of the flocculant is reduced due to too small addition of the initiator.
3. The centrifugate flocculated by the flocculating agent can be reused for preparing the oil-based drilling fluid, so that the utilization rate of the centrifugate of the oil-based drilling fluid is improved.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, which are only a part of the embodiments of the present invention, but not all of the embodiments. The experimental technical methods and scientific terms used in the examples have the same meanings as commonly understood by a person of ordinary skill in the art without specific descriptions. The involved experimental consumables and reagents are generally available from commercial sources if no special remarks exist.
The styrene used in the examples and comparative examples was pretreated styrene by the following pretreatment method:
placing a styrene monomer in a separating funnel, then adding a 10% NaOH aqueous solution into the funnel, screwing a piston to repeatedly shake until the NaOH solution turns red until the color is not deepened; and washing for 3 times to remove the polymerization inhibitor in the styrene monomer, wherein in each washing process, the mass ratio of the styrene to the NaOH aqueous solution is 1.2.
Example 1
A preparation method of an oil-based drilling fluid centrifugate flocculant comprises the following steps:
(1) Adding 10g of styrene, 15g of 4-vinylpyridine and 21g of dimethyldiallylammonium chloride into a three-neck flask filled with a mixed solution of 20g of ethanol and 80g of toluene, magnetically stirring to uniformly disperse the styrene, and then heating to 65 ℃;
(2) When the temperature reaches 65 ℃, 0.25g of benzoyl peroxide is added into the solution, and the reaction is continued for 12 hours at 65 ℃;
(3) After the reaction is finished, cooling to room temperature, precipitating an oil-soluble polymer with methanol (the volume ratio of methanol to the reaction liquid is 5.
Example 2
A preparation method of an oil-based drilling fluid centrifugate flocculant comprises the following steps:
(1) Adding 12g of styrene, 14g of 4-vinylpyridine and 20g of dimethyl diallyl ammonium chloride into a three-neck flask filled with a mixed solution of 30g of ethanol and 70g of toluene, magnetically stirring to uniformly disperse the styrene, and then heating to 65 ℃;
(2) When the temperature reaches 65 ℃, adding 0.3g of azobisisobutyronitrile into the solution, and continuously reacting for 12 hours at 65 ℃;
(3) After the reaction is finished, cooling to room temperature, precipitating an oil-soluble polymer with methanol (the volume ratio of methanol to the reaction liquid is 5.
Example 3
A preparation method of an oil-based drilling fluid centrifugate flocculant comprises the following steps:
(1) Adding 15g of styrene and 15g of 4-vinylpyridine and 22g of dodecyl methyl diallyl ammonium chloride into a three-neck flask filled with a mixed solution of 30g of ethanol and 70g of toluene, uniformly dispersing the mixture by magnetic stirring, and then heating to 70 ℃;
(2) When the temperature reaches 70 ℃, 0.3g of tert-butyl hydroperoxide is added into the solution, and the reaction is continued for 15h at 70 ℃;
(3) After the reaction is finished, cooling to room temperature, precipitating an oil-soluble polymer with methanol (the volume ratio of methanol to the reaction liquid is 4.
Example 4
A preparation method of an oil-based drilling fluid centrifugate flocculant comprises the following steps:
(1) Adding 6g of styrene, 16g of 4-vinylpyridine and 24g of dodecyl methyl diallyl ammonium chloride into a three-neck flask filled with a mixed solution of 50g of ethanol and 50g of toluene, magnetically stirring to uniformly disperse the styrene and the 4-vinylpyridine, and then heating to 75 ℃;
(2) When the temperature reaches 75 ℃, adding 0.3g of azobisisobutyronitrile into the solution, and continuously reacting for 12 hours at 75 ℃;
(3) After the reaction is finished, cooling to room temperature, precipitating an oil-soluble polymer by using methanol (the volume ratio of the methanol to the reaction liquid is 3.
Example 5
A preparation method of an oil-based drilling fluid centrifugate flocculant comprises the following steps:
(1) Taking 8g of styrene, 12g of 4-vinylpyridine and 20g of acryloyloxyethyltrimethyl ammonium chloride, adding the styrene, the 4-vinylpyridine and the acryloyloxyethyltrimethyl ammonium chloride into a three-neck flask filled with a mixed solution of 30g of ethanol and 70g of toluene, stirring by magnetic force to disperse the styrene and the toluene uniformly, and then heating to 70 ℃;
(2) When the temperature reaches 70 ℃, adding 0.25g of tert-butyl hydroperoxide into the solution, and continuously reacting for 16h at 70 ℃;
(3) After the reaction is finished, cooling to room temperature, precipitating an oil-soluble polymer by using methanol (the volume ratio of the methanol to the reaction liquid is 3.
Example 6
A preparation method of an oil-based drilling fluid centrifugate flocculant comprises the following steps:
(1) Adding 14g of styrene, 15g of 4-vinylpyridine and 18g of acryloyloxyethyl trimethyl ammonium chloride into a three-neck flask filled with a mixed solution of 30g of ethanol and 70g of toluene, magnetically stirring to uniformly disperse the mixture, and then heating to 65 ℃;
(2) When the temperature reaches 65 ℃, adding 0.3g of azobisisobutyronitrile into the solution, and continuously reacting for 16 hours at 65 ℃;
(3) After the reaction is finished, cooling to room temperature, precipitating an oil-soluble polymer with methanol (the volume ratio of methanol to the reaction liquid is 4.
Comparative example 1
A flocculant for an oil based drilling fluid centrate is prepared as described in example 1, except that: 50g of styrene was taken in the step (1), and the other conditions were the same as in example 1 to obtain a flocculant D1.
Comparative example 2
A flocculant for an oil-based drilling fluid centrate is prepared as described in example 1, except that: 4-vinylpyridine was not added in step (1), and the other conditions were the same as in example 1 to obtain flocculant D2.
Comparative example 3
A flocculant for an oil based drilling fluid centrate is prepared as described in example 1, except that: dimethyl diallyl ammonium chloride is not added in the step (1), and the other conditions are the same as those in the example 1, so that the flocculant D3 is obtained.
Comparative example 4
A flocculant for an oil-based drilling fluid centrate is prepared as described in example 1, except that: 0.1g of benzoyl peroxide was added in step (2), and the other conditions were the same as in example 1, to obtain flocculant D4.
Test examples
The flocculants prepared in examples 1-6 and comparative examples 1-4 were used to treat oil-based drilling fluid centrates to evaluate the performance of the flocculants for oil-based drilling fluid centrates provided by the present invention. In the following test examples, the following test examples were carried out,
the solid phase median particle size of the drilling fluid centrifugate is measured by a focused beam reflectometer (Mettler-Toolido, particle track G600B);
the plastic viscosity (mPa · s), dynamic shear force (Pa) and initial and final shear (Pa) of the drilling fluid centrifugate are measured by a six-speed viscometer according to the method specified in GB/T16783.2-2012;
the density of the drilling fluid centrifugate and the poor solid content of the drilling fluid centrifugate are determined according to the method specified in GB/T16783.2-2012, and the poor solid content refers to the volume content under the condition that no special description is given;
the six-speed viscometer is manufactured by Qingdao Tongchun petroleum instrument GmbH and has the model of ZNN-D6B;
the manufacturer of the low-speed stirrer is Qingdao Tongchun petroleum instrument company, type D90;
the manufacturer of the centrifuge was Hunan instruments laboratory Instrument development Co., ltd, model TG16-WS.
Oil-based drilling fluid centrifugate sample S0:
in the test example, the oil-based drilling fluid centrifugate S0 sampling Szechwan Wigner block is an oil-based drilling fluid centrifugate sample obtained by processing through three-level solid control equipment including a vibrating screen, a drying machine and a centrifugal machine, and the sample is tested as follows.
1. Solid phase particle size test after treatment of drilling fluid centrifugate sample by adding flocculant
0.1g of the flocculant prepared in the examples 1 to 5 and the comparative examples 1 to 4 of the invention is added into 100mL of the oil-based drilling fluid centrifugate sample respectively, and the mixture is stirred for 5min at 500r/min by using a low-speed stirrer to obtain the flocculated drilling fluid centrifugate (the drilling fluid centrifugate flocculated by adding the flocculant of the examples 1 to 6 of the invention is respectively marked as BS1 to BS6, the drilling fluid centrifugate flocculated by adding the flocculant of the comparative examples 1 to 4 of the invention is respectively marked as BD1 to BD4, the same applies below), and the focused beam reflectometer is used for testing the solid phase particle size median of the drilling fluid. S0 is used as a blank control group, no flocculating agent is added, and other test conditions are completely the same as those of other test groups. The test results are shown in table 1.
TABLE 1 influence of flocculants on poor solid phase particle size of oil-based drilling fluid centrifugate
As can be seen from Table 1, after the flocculant provided by the invention is added into an oil-based drilling fluid centrifugate sample, the solid phase median particle size in the drilling fluid centrifugate is greatly increased, and is increased to more than 67 micrometers from 32 micrometers. Wherein, the embodiment 1-3 is in the optimal range of the invention, the effect is optimal, and the solid phase median diameter of the drilling fluid centrifugate after flocculation treatment is improved to over 86 μm. The flocculating agent provided by the invention has an obvious flocculation effect on micro-scale poor solid-phase particles in an oil-based drilling fluid centrifugate sample.
2. Rheological property test of drilling fluid centrifugate sample after flocculant addition treatment
100mL of the solution with the density of 1.80g/cm is taken 3 0.1g of the flocculant prepared in the examples 1-6 and the comparative examples 1-4 of the invention is added into the oil-based drilling fluid centrifugate in multiple parts, and simultaneously a low-speed stirrer is used for stirring at 500r/min for 5min to obtain the centrifugate after flocculation treatment, and a centrifuge is used for centrifuging at 3000 r/min for 5min, and then the upper layer liquid is taken to test the rheological parameters. S0 as blank control group, without flocculant, other testsThe conditions were identical to the other test groups. The test results are shown in table 2.
TABLE 2 centrifuge rheology Performance test after flocculation
As can be seen from Table 2, after the flocculant provided by the embodiment of the invention is added into an oil-based drilling fluid centrifugate sample and the oil-based drilling fluid centrifugate sample is centrifuged, the plastic viscosity, the dynamic shear force and the initial/final shear of the drilling fluid are obviously reduced. This is because the poor solid phase inside the drilling fluid reduces friction between the drilling fluid particles, manifested as a decrease in viscosity, after the poor solid phase is removed.
3. Testing density and inferior solid phase content of centrifugate after adding flocculant into drilling fluid centrifugate sample for treatment
0.1g of the flocculant prepared in the examples 1-6 and the comparative examples 1-4 of the invention is respectively added into 100mL of oil-based drilling fluid centrifugate samples, and simultaneously, a low-speed stirrer is used for stirring at 500r/min for 5min to obtain the drilling fluid centrifugate after flocculation treatment, and a centrifuge is used for centrifuging at 3000 r/min for 5min, and then the upper layer liquid is taken to test the density and the content of poor solid phase. S0 is used as a blank control group, no flocculating agent is added, and other test conditions are completely the same as those of other test groups. The test results are shown in table 3.
TABLE 3 Density and inferior solid content test of flocculated centrifugate
As can be seen from Table 3, the density and poor solid phase of the drilling fluid are both obviously reduced after the flocculant provided by the invention is added into the centrifugate sample of the oil-based drilling fluid and the oil-based drilling fluid is centrifuged. The density of the centrifugate treated by the flocculant is 1.80g/cm 3 Reduced to 1.13g/cm 3 The content of the poor solid phase is reduced from 31 percent to 9 percent, which shows that the flocculant provided by the invention has obvious flocculation removal effect on the micro-scale poor solid phase in the oil-based drilling fluid centrifugal liquid sample.
4. Influence of flocculant-treated drilling fluid centrifugate on rheological property of oil-based drilling fluid after re-slurry preparation
And (3) taking the prepared oil-based drilling fluid as a blank sample, respectively adding flocculating agent-treated oil-based drilling fluid centrifugates BS1-BS6, and BD1-BD4 for slurry preparation in the ratio of 1. Wherein, the blank oil-based drilling fluid is 50 parts by weight, and the drilling fluid centrifugate is 50 parts by weight after being processed by the flocculant.
The formula of the oil-based drilling fluid comprises the following components: 100 parts by weight of white oil, 3 parts by weight of a primary emulsifier OME (available from Shandong Shunyuan oil science and technology Co., ltd.) +3 parts by weight of a secondary emulsifier OME-2 (available from Shandong Shunyuan oil science and technology Co., ltd.) + increasing the weight of the mixture to a density of 2.3g/cm using barite 3 。
Respectively mixing 50 parts by weight of flocculant-treated oil-based drilling fluid centrifugates BS1-BS6 and BD1-BD4 with 50 parts by weight of the drilling fluid to simulate the recycling process of the oil-based drilling fluid centrifugate. Then stirred at high speed for 20 minutes, then the test object is put into an aging tank and hot rolled at 180 ℃ for 16 hours, cooled to room temperature, transferred into a stirring cup and stirred at high speed for 20 minutes, the temperature of the drilling fluid is kept at 65 ℃, and the rheological property is measured, and the result is shown in Table 4.
TABLE 4 evaluation of rheological Properties of drilling fluids after repulping
As can be seen from Table 4, when the flocculant-treated centrifugating fluid provided by the invention is added into an oil-based drilling fluid sample, the plastic viscosity, the dynamic shear force and the initial and final shear of the obtained drilling fluid are basically kept unchanged. The flocculant provided by the invention is added into the oil-based drilling fluid centrifugate, so that the poor solid phase is removed by solid control equipment due to the increase of the particle size through flocculation. After the poor solid phase is removed, the solid phase content in the drilling fluid centrifugate is reduced, so that the friction among drilling fluid particles is reduced, and the viscosity is basically kept unchanged.
What has been described above includes examples of one or more embodiments. Of course, one of ordinary skill in the art will recognize that further combinations and permutations of the various embodiments are possible. Accordingly, the embodiments described herein are intended to embrace all such alterations, modifications and variations that fall within the scope of the appended claims. Furthermore, to the extent that the term "includes" is used in either the detailed description or the claims, such term is intended to be inclusive in a manner similar to the term "comprising" as "comprising" is interpreted when employed as a transitional word in a claim. Furthermore, any use of the term "or" in the specification of the claims is intended to mean a "non-exclusive or".
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A preparation method of an oil-based drilling fluid centrifugate flocculant comprises the following steps:
adding pretreated styrene, 4-vinylpyridine and cationic monomer into a solvent, stirring to uniformly disperse the styrene, the 4-vinylpyridine and the cationic monomer, and then heating to a reaction temperature; then adding an initiator to carry out constant temperature reaction; and after the reaction is finished, cooling to room temperature, adding methanol into the obtained reaction liquid to separate out a polymer, and then filtering and drying to obtain the oil-based drilling fluid centrifugal liquid flocculant.
2. The preparation method of the oil-based drilling fluid centrifugate flocculant according to claim 1, wherein the solvent is a mixed solution of ethanol and toluene, and the mass ratio of ethanol to toluene in the mixed solution is 1.
3. The preparation method of the flocculant of oil-based drilling fluid centrifugate according to claim 1, wherein the styrene is pretreated by the following steps: washing styrene for 3 times by using NaOH aqueous solution with the mass fraction of 10-20%; in each washing process, the mass ratio of the styrene to the NaOH aqueous solution is 1.
4. The preparation method of the flocculant of oil-based drilling fluid centrifugate according to claim 1, wherein the cationic monomer is one or a combination of more than two of dimethyldiallylammonium chloride, dodecylmethyldiallylammonium chloride and acryloyloxyethyltrimethylammonium chloride.
5. The preparation method of the flocculant of the oil-based drilling fluid centrifugate according to the claim 1, which is characterized in that the pretreated styrene comprises 6 to 16 parts by weight of 4-vinylpyridine 12 to 18 parts by weight of cationic monomer 18 to 26 parts by weight of solvent 100 parts by weight; preferably, the pretreated styrene is 8 to 14 parts, the 4-vinylpyridine is 14 to 16 parts, and the cationic monomer is 20 to 24 parts, based on 100 parts by weight of the solvent.
6. The method for preparing the flocculant of oil-based drilling fluid centrifugate according to claim 1, wherein the initiator is one of benzoyl peroxide, azobisisobutyronitrile and tert-butyl hydroperoxide; the mass of the initiator is 0.3-0.8% of the total mass of the pretreated styrene, the 4-vinylpyridine and the cationic monomer.
7. The preparation method of the flocculant of oil-based drilling fluid centrifugate according to claim 1, wherein the reaction temperature is 60-80 ℃, and more preferably 65-75 ℃; the constant temperature reaction time is 10-20h, and the preferable time is 12-18h;
preferably, the volume ratio of the methanol to the reaction liquid is 3-5; the drying is vacuum drying at 50-70 deg.C for 10-15h.
8. The flocculant of the oil-based drilling fluid centrifugate is characterized by being prepared by the preparation method of any one of claims 1 to 7.
9. Use of the oil-based drilling fluid centrate flocculant of claim 8 in the recovery of oil-based drilling fluid oily drill cuttings centrate flocculation.
10. The application of claim 9, wherein the specific application method is as follows: under the condition of stirring, adding the prepared oil-based drilling fluid centrifugate flocculant into the oil-containing drilling cuttings centrifugate of the oil-based drilling fluid, transferring the oil-based drilling fluid centrifugate flocculant into a centrifuge for centrifugation after uniform dispersion, and collecting the centrifuged centrifugate to realize recycling of the oil-containing drilling cuttings centrifugate; the stirring rotating speed is 500-3000rpm, the mass of the oil-based drilling fluid centrifugate flocculant is 0.1-5% of the mass of the oil-based drilling fluid oily drilling cutting centrifugate, and the centrifugation rotating speed is 1500-3500rpm.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4455240A (en) * | 1981-12-15 | 1984-06-19 | Calgon Corporation | Ampholytic polymers for use as filtration control aids in drilling muds |
| CN113292731A (en) * | 2021-07-08 | 2021-08-24 | 中国石油大学(华东) | Flocculant for removing rock debris of oil-based drilling fluid and preparation method and application thereof |
| CN113861341A (en) * | 2021-10-18 | 2021-12-31 | 北京石油化工学院 | Oil-soluble flocculant special for oil-based drilling fluid and preparation method thereof |
| CN114605582A (en) * | 2022-03-02 | 2022-06-10 | 中国石油集团安全环保技术研究院有限公司 | Oil-based drilling fluid flocculant and preparation method and application thereof |
| CN114621373A (en) * | 2021-06-10 | 2022-06-14 | 中国石油天然气集团有限公司 | Flocculant for oil-based drilling fluid and preparation method and application thereof |
-
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- 2022-10-13 CN CN202211254418.6A patent/CN115626963B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4455240A (en) * | 1981-12-15 | 1984-06-19 | Calgon Corporation | Ampholytic polymers for use as filtration control aids in drilling muds |
| CN114621373A (en) * | 2021-06-10 | 2022-06-14 | 中国石油天然气集团有限公司 | Flocculant for oil-based drilling fluid and preparation method and application thereof |
| CN113292731A (en) * | 2021-07-08 | 2021-08-24 | 中国石油大学(华东) | Flocculant for removing rock debris of oil-based drilling fluid and preparation method and application thereof |
| CN113861341A (en) * | 2021-10-18 | 2021-12-31 | 北京石油化工学院 | Oil-soluble flocculant special for oil-based drilling fluid and preparation method thereof |
| CN114605582A (en) * | 2022-03-02 | 2022-06-10 | 中国石油集团安全环保技术研究院有限公司 | Oil-based drilling fluid flocculant and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117164752A (en) * | 2023-11-03 | 2023-12-05 | 中石化西南石油工程有限公司 | Flocculant for oil-based drilling fluid and preparation method thereof |
| CN117164752B (en) * | 2023-11-03 | 2024-02-27 | 中石化西南石油工程有限公司 | Flocculant for oil-based drilling fluid and preparation method thereof |
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