CN104804714B - Receive crystalline cellulose as the application of fluid loss additive for boring fluid and drilling fluid - Google Patents
Receive crystalline cellulose as the application of fluid loss additive for boring fluid and drilling fluid Download PDFInfo
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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
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/20—Natural organic compounds or derivatives thereof, e.g. polysaccharides or lignin derivatives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/20—Natural organic compounds or derivatives thereof, e.g. polysaccharides or lignin derivatives
- C09K8/206—Derivatives of other natural products, e.g. cellulose, starch, sugars
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/08—Fiber-containing well treatment fluids
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/10—Nanoparticle-containing well treatment fluids
Abstract
The present invention relates to and receive crystalline cellulose as the application of fluid loss additive for boring fluid and drilling fluid.This drilling fluid contains fluid loss agent, and wherein said fluid loss agent is for receiving crystalline cellulose.Crystalline cellulose of receiving provided by the invention, as fluid loss additive for boring fluid, not only has lower-cost feature, also has excellent filtrate loss controllability.
Description
Technical field
The present invention relates to and receive crystalline cellulose as the application of fluid loss additive for boring fluid and drilling fluid.
Background technology
The problem maintaining wellbore stability is a global problem of drilling well industry, and this problem in the world many oil fields all exists, and never can be solved very well.Along with China's oil-gas exploration and development target is further towards being imbedded in the very complicated Deep Oil And Gas Exploration resource of geologic condition and the unconventional resource such as coal-seam gas, shale gas, a wellbore stability difficult problem is often run in drilling process, this will cause Tail Pipe For Complicated Deep Wells and shale gas horizontal well drilling speed is slow, complex accident is many, drilling period is long, cost is high, and these have had a strong impact on, and China's hydrocarbon resources is important takes over district's exploratory development process.
In drilling process, the borehole well instability accident of 90% occurs in mud shale stratum, and in mud shale, clay causes mud shale to disperse, peel off because of hydration swelling is the most basic factor causing borehole well instability.If can the hole of shutoff mud shale nano-micrometer level and microfracture, then the intrusion of free water in drilling fluid can not only be avoided to cause shale hydration to disperse, drilling liquid pressure can also be stoped to transmit to depths, stratum, thus high degree improves borehole wall stability.
But mud shale stratum mostly is nano level hole, rate of permeation is extremely low, thus causes conventional drilling liquid cannot form thicker filter cake in mud shale borehole wall surface.In addition the filter cake particle that the drilling fluid adding traditional fluid loss agent is formed is comparatively large, and filter cake is fine and close not, is difficult to effectively stop free water to invade mud shale.
In order to stop mud filtrate invasion mud shale stratum to cause borehole well instability, M-I company describes nano-graphene or its derivative nano material for shutoff mud shale microporosity and maintains the application of mud shale wellbore stability in patent US2013/0264121A1.But, Graphene and derivant material cost very expensive, and be still difficult to industrial production in enormous quantities at present.
Summary of the invention
The object of the invention is to overcome the defect of fluid loss additive for boring fluid high cost in prior art, provide and receive crystalline cellulose as the application of fluid loss additive for boring fluid and drilling fluid.
The present inventor surprisingly finds, crystalline cellulose particle is received as fluid loss additive for boring fluid using what there is specific dimensions, carbon nanotube compared to existing technology, Graphene class fluid loss agent, crystalline cellulose of receiving not only has inexpensive feature, thin and the filter cake of densification can be formed in borehole wall surface after fluid loss agent and drilling fluid mixed using receiving crystalline cellulose, thus can significantly improve the leak-off building capacity of drilling fluid, thus improve filtrate reducing effect.
The invention provides and receive the application of crystalline cellulose as fluid loss additive for boring fluid.
Present invention also offers a kind of drilling fluid, this drilling fluid contains fluid loss agent, and wherein, described fluid loss agent is for receiving crystalline cellulose.
Preferably, the median size of crystalline cellulose received described in is 100-600nm.
Provided by the invention there is specific dimensions receive crystalline cellulose as fluid loss additive for boring fluid, not only there is lower-cost feature, also there is excellent filtrate loss controllability.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides and receive the application of crystalline cellulose as fluid loss additive for boring fluid.
In order to obtain more excellent filtrate loss controllability, described in receive the median size of crystalline cellulose and be preferably 100-600nm, be more preferably 150-320nm.
Preferably, crystalline cellulose of receiving described in is bar-shaped.
In the present invention, Japanese JEOL company model is adopted to be that the transmission electron microscope (TEM) of JEM-2100 measures and receives the microscopic pattern of crystalline cellulose particle and median size.Sample preparation methods: by be diluted to concentration be 0.1 % by weight the aqueous dispersions of crystalline cellulose received drip on the micro-grid of copper that carbon film covers, and to dry with infrared lamp.
Application according to the present invention, can with reference to prior art as the application method of fluid loss additive for boring fluid using receiving crystalline cellulose, and such as the drilling fluid containing fluid loss agent can be applied in drilling process, wherein said fluid loss agent is for receiving crystalline cellulose.
As long as receive crystalline cellulose particle and namely can be used as fluid loss additive for boring fluid although add in described drilling fluid and play excellent filtrate reducing effect, but under preferable case, in order to realize goal of the invention of the present invention better, relative to the described drilling fluid of 100 weight parts, the content of described fluid loss agent is 0.1-5 weight part, is more preferably 0.2-1 weight part.
In the present invention, drilling fluid refers in drilling process, the circulation flushing medium used in hole.
According to the present invention, described in receive crystalline cellulose and can be obtained by the mode be purchased, also can be prepared by method well-known to those skilled in the art, such as, described in receive crystalline cellulose and be prepared by the following method:
(1) Microcrystalline Cellulose is mixed with acid solution;
(2) mixture that step (1) obtains is contacted with water, then the product of gained is carried out solid-liquid separation.
According to aforesaid method, in step (1), be the noncrystalline domain making acid solution infiltrate Microcrystalline Cellulose by the object that Microcrystalline Cellulose mixes with acid solution, to accelerate the hydrolysis of Microcrystalline Cellulose.In the present invention, the condition of described mixing comprises: the temperature of mixing is 30-70 DEG C, is preferably 35-60 DEG C; The time of mixing is 1-15h, is preferably 3-10h.Described mixing realizes preferably by homogenizer, and rotating speed can turn/min for 100-300.
According to aforesaid method, in step (1), the weight ratio of described Microcrystalline Cellulose and described acid solution can change in wider scope, as long as Microcrystalline Cellulose can be made to be hydrolyzed.Usually, the weight ratio of described Microcrystalline Cellulose and described acid solution can be 1:20-40, is preferably 1:20-30.The concentration of described acid solution can be 30-80 % by weight, is preferably 50-70 % by weight.
According to aforesaid method, the acid in described acid solution can be the mineral acid that can infiltrate the non-crystalline region of Microcrystalline Cellulose of various routine or organic acid.In the present invention, described mineral acid can be conventional various mineral acids, such as, can be one or more in hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid; Described organic acid can be conventional various organic acids, and such as carbonatoms is unitary or the binary organic carboxyl acid of 1-5, is specifically as follows one or more in formic acid, acetic acid, tartrate and citric acid.
In the present invention, described Microcrystalline Cellulose can be obtained by the mode be purchased.In order to obtain there is specific dimensions receive crystalline cellulose particle, under preferable case, the median size of described microcrystalline cellulose crude granule is 20-80 μm, is more preferably 20-50 μm.
According to aforesaid method, in step (2), mixture step (1) obtained and the object that water carries out contacting are the hydrolysis reaction stopping Microcrystalline Cellulose with water.Relative to the Microcrystalline Cellulose of 100 weight parts, the consumption of water can be 2000-7500 weight part, is preferably 4000-7500 weight part.
According to aforesaid method, the method for solid-liquid separation described in step (2) can be the solid-liquid separating method of various routine in this area, such as, can be filtering separation and/or centrifugation.Under preferable case, described solid-liquid separation is centrifugation.In the present invention, to described centrifugal condition, there is no particular limitation, obtains crystal and liquid phase as long as gained suspension can be separated.The condition of centrifugation comprises: centrifugal rotating speed is that 3000-11000 turns/min, is preferably 6000-11000 and turns/min; Centrifugation time is 5-30min, is preferably 10-20min.
In order to avoid the acid of remnants is on the impact of follow-up filtrate reducing effect, aforesaid method preferably includes solid water centrifugation obtained and carries out washing until the pH value of liquid of centrifugal gained is 6-7, then carries out drying.The condition of described drying comprises: dry temperature is 100-110 DEG C, and the dry time is 8-12h.
In the present invention, described drilling fluid can be various drilling fluid known in the art, and consider that receiving crystalline cellulose can play the effect of better fluid loss additive for boring fluid, under preferable case, described drilling fluid is water-base drilling fluid.
In the present invention, described water-base drilling fluid adds for main matrix the heterogeneous dispersion system that various additive forms with water.The various water-base drilling fluids that described water-base drilling fluid can be well known to those skilled in the art, such as described water-base drilling fluid can one or more for being selected from water, Repone K-polyglycol drilling fluid, silicone drilling fluid and cationic drilling fluid.Wherein, the various water that described water can be well known to those skilled in the art can be such as one or more in fresh water (tap water), seawater and salt solution; Various Repone K-polyglycol drilling fluid that described Repone K-polyglycol drilling fluid can be well known to those skilled in the art can be such as one or more in Repone K-PEG drilling fluid, Repone K-polypropylene glycol drilling fluid, Repone K-ethylene glycol/propylene glycol copolymers drilling fluid, Repone K-polyglycerol drilling fluid and Repone K-polyethylene glycol drilling fluid; The various silicone drilling fluid that described silicone drilling fluid can be well known to those skilled in the art, the organosilicon in described silicone drilling fluid can one or more for being selected from methyl silicon sodium alcoholate, methyl silanol potassium and organic silicone potassium humate.The various cationic drilling fluid that described cationic drilling fluid can be well known to those skilled in the art, positively charged ion in described cationic drilling fluid can one or more for being selected from 2,3-epoxypropyltrimethylchloride chloride, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and cationic polyacrylamide.
In the present invention, in order to obtain better drilling well effect, various additive well-known to those skilled in the art can also in described drilling fluid, be added.Such as described additive can one or more for being selected from soil with slurry, alkaline carbonate, inhibitor, tackifier, viscosity-depression agent, weighting agent, coating agent and lubricant.
In the present invention, the add-on of described additive is not particularly limited, the various add-ons can selected according to the effect that will reach for those skilled in the art, such as relative to the described drilling fluid of 100 weight parts, the content of described soil with slurry can be 2-4 weight part, the content of described alkaline carbonate can be 0.1-1 weight part, the content of described inhibitor can be 0.2-3 weight part, the content of described tackifier can be 0.2-1 weight part, the content of described viscosity-depression agent can be 0.2-1 weight part, the content of described weighting agent can be 0.2-3 weight part, the content of described coating agent can be 0.2-1 weight part, the content of described lubricant can be 0.1-2 weight part.
In the present invention, described soil with slurry is preferably wilkinite.Described wilkinite refers to montmorillonite to be the clay of main mineral constituent, and it has the effect of giving drilling fluid and gluing shear force and leak-off building capacity, such as, can be sodium bentonite and/or calcium-base bentonite, preferably sodium bentonite; Described alkaline carbonate has the effect improving wilkinite pulping performance, can be sodium carbonate, salt of wormwood and Quilonum Retard, is preferably sodium carbonate; Described inhibitor can be one or more in Repone K, small cation inhibitor and polyether diamine, and wherein, described small cation inhibitor can be 2,3-epoxypropyltrimethylchloride chloride; Described tackifier can be one or more in xanthan gum natural gum, xanthan gum, carboxymethyl starch, Walocel MT 20.000PV, Natvosol, carboxymethyl cellulose, Polyanionic Cellulose (the water-soluble cellulose ether analog derivative that natural cellulose is obtained through chemical modification) and synthesis tackifier (partially hydrolyzed polyacrylamide); Described viscosity-depression agent can be one or more in feero-chromo-lignosulfonate, sodium polyacrylate, methyl silicon sodium alcoholate and Sulfonated Copolymer of Styrene and Maleic Anhydride; Described weighting agent can be one or more in the mixture of powdered iron ore, Paris white, barite and rhombohedral iron ore and lead glance powder; Described coating agent can be one or more in partially hydrolyzed polyacrylamide (aqueous or powdery), cationic polyacrylamide and polymerize aluminum chloride; Described lubricant is one or more in nonionogenic tenside, graphite and polymeric alcohol.
The present invention also provides a kind of drilling fluid, and this drilling fluid contains fluid loss agent, and wherein, described fluid loss agent is for receiving crystalline cellulose.
In order to obtain more excellent filtrate loss controllability, described in receive the median size of crystalline cellulose particle and be preferably 100-600nm, be more preferably 150-320nm.
Preferably, crystalline cellulose of receiving described in is bar-shaped.
As long as receive crystalline cellulose particle and namely can be used as fluid loss additive for boring fluid although add in described drilling fluid and play excellent filtrate reducing effect, but under preferable case, in order to realize goal of the invention of the present invention better, relative to the described drilling fluid of 100 weight parts, the content of described fluid loss agent is 0.1-5 weight part, is more preferably 0.2-1 weight part.
In the present invention, the definition of described drilling fluid with describe identical above, do not repeat them here.
According to drilling fluid of the present invention, described in receive crystalline cellulose and can be obtained by the mode be purchased, also can be prepared by method well-known to those skilled in the art, such as, described in receive crystalline cellulose and be prepared by the following method:
(1) Microcrystalline Cellulose is mixed with acid solution;
(2) mixture that step (1) obtains is contacted with water, then the product of gained is carried out solid-liquid separation.
According to aforesaid method, in step (1), be the noncrystalline domain making acid solution infiltrate Microcrystalline Cellulose by the object that Microcrystalline Cellulose mixes with acid solution, to accelerate the hydrolysis of Microcrystalline Cellulose.In the present invention, the condition of described mixing comprises: the temperature of mixing is 30-70 DEG C, is preferably 35-60 DEG C; The time of mixing is 1-15h, is preferably 3-10h.Described mixing realizes preferably by homogenizer, and rotating speed can turn/min for 100-300.
According to aforesaid method, in step (1), the weight ratio of described Microcrystalline Cellulose and described acid solution can change in wider scope, as long as Microcrystalline Cellulose can be made to be hydrolyzed.Usually, the weight ratio of described Microcrystalline Cellulose and described acid solution can be 1:20-40, is preferably 1:20-30.The concentration of described acid solution can be 30-80 % by weight, is preferably 50-70 % by weight.
According to aforesaid method, the acid in described acid solution can be the mineral acid that can infiltrate the non-crystalline region of Microcrystalline Cellulose of various routine or organic acid.In the present invention, described mineral acid can be conventional various mineral acids, such as, can be one or more in hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid; Described organic acid can be conventional various organic acids, and such as carbonatoms is unitary or the binary organic carboxyl acid of 1-5, is specifically as follows one or more in formic acid, acetic acid, tartrate and citric acid.
In the present invention, described Microcrystalline Cellulose can be obtained by the mode be purchased.In order to obtain there is specific dimensions receive crystalline cellulose particle, under preferable case, the median size of described microcrystalline cellulose crude granule is 20-80 μm, is more preferably 20-50 μm.
According to aforesaid method, in step (2), mixture step (1) obtained and the object that water carries out contacting are the hydrolysis reaction stopping Microcrystalline Cellulose with water.Relative to the Microcrystalline Cellulose of 100 weight parts, the consumption of water can be 2000-7500 weight part, is preferably 4000-7500 weight part.
According to aforesaid method, the method for solid-liquid separation described in step (2) can be the solid-liquid separating method of various routine in this area, such as, can be filtering separation and/or centrifugation.Under preferable case, described solid-liquid separation is centrifugation.In the present invention, to described centrifugal condition, there is no particular limitation, obtains crystal and liquid phase as long as gained suspension can be separated.The condition of centrifugation comprises: centrifugal rotating speed is that 3000-11000 turns/min, is preferably 6000-11000 and turns/min; Centrifugation time is 5-30min, is preferably 10-20min.
In order to avoid the acid of remnants is on the impact of follow-up filtrate reducing effect, aforesaid method preferably includes solid water centrifugation obtained and carries out washing until the pH value of liquid of centrifugal gained is 6-7, then carries out drying.The condition of described drying comprises: dry temperature is 100-110 DEG C, and the dry time is 8-12h.
In the present invention, described drilling fluid can be various drilling fluid known in the art, and consider that receiving crystalline cellulose can play the effect of better fluid loss additive for boring fluid, under preferable case, described drilling fluid is water-base drilling fluid.
In the present invention, the kind of described water-base drilling fluid with describe consistent above, do not repeat them here.
In the present invention, in order to obtain better drilling well effect, various additive well-known to those skilled in the art can also in described drilling fluid, be added.Such as described additive can one or more for being selected from soil with slurry, alkaline carbonate, inhibitor, tackifier, viscosity-depression agent, weighting agent, coating agent and lubricant.
In the present invention, the add-on of described additive is not particularly limited, the various add-ons can selected according to the effect that will reach for those skilled in the art, such as relative to the described drilling fluid of 100 weight parts, the content of described soil with slurry can be 2-4 weight part, the content of described alkaline carbonate can be 0.1-1 weight part, the content of described inhibitor can be 0.2-3 weight part, the content of described tackifier can be 0.2-1 weight part, the content of described viscosity-depression agent can be 0.2-1 weight part, the content of described weighting agent can be 0.2-3 weight part, the content of described coating agent can be 0.2-1 weight part, the content of described lubricant can be 0.1-2 weight part.
The kind of described soil with slurry, alkaline carbonate, inhibitor, tackifier, viscosity-depression agent, weighting agent, coating agent and lubricant with describe identical above, do not repeat them here.
Drilling fluid in the present invention may be used for various Oil/gas Well, such as straight well, orientation well, extended reach well, horizontal well etc.
Below will be described the present invention by embodiment.
It should be noted that, receiving the effect of crystalline cellulose as fluid loss additive for boring fluid, in an embodiment of the present invention, with fresh water (tap water) Simulated Water base drilling fluid for the ease of measuring.
In following preparation example, receive the calculation formula of productive rate of crystalline cellulose:
In following preparation example, Japanese JEOL company model is adopted to be that the transmission electron microscope (TEM) of JEM measures and receives the microscopic pattern of crystalline cellulose particle and median size.The preparation method of sample: by be diluted to concentration be 0.1 % by weight the aqueous dispersions of crystalline cellulose received drip on the micro-grid of copper that carbon film covers, and to dry with infrared lamp.
Preparation example 1-7 is for illustration of the cellulosic preparation method of nanocrystal provided by the invention.
Preparation example 1
(1) 40g Microcrystalline Cellulose (purchased from Hubei Zhong Liao Chemical Co., Ltd., the median size of particle is 20 μm) being added concentration is in the 700mL aqueous sulfuric acid of 64 % by weight, and with the rotating speed high-speed stirring 3h of 250 turns/min at 45 DEG C;
(2) 3L deionized water is added to stop the hydrolysis reaction of Microcrystalline Cellulose in the mixture obtained to step (1); By the suspension centrifugal 20min under 11000r/min obtained, then by the solid deionized water wash of centrifugal gained for several times, the pH value of the clear liquid obtained until centrifugal is 7; By the solid dry 12h at 105 DEG C cleaned, namely obtain the crystalline cellulose N1 that receives of 35.28g, productive rate is 88.2%.Measuring product by transmission electron microscope (TEM), to receive the median size of crystalline cellulose be 239nm, and crystalline cellulose of receiving is bar-shaped.
Preparation example 2
(1) 40g Microcrystalline Cellulose (purchased from Hubei Zhong Liao Chemical Co., Ltd., the median size of particle is 80 μm) being added concentration is in the 700mL aqueous sulfuric acid of 64 % by weight, and with the rotating speed high-speed stirring 3h of 250 turns/min at 45 DEG C;
(2) 3L deionized water is added to stop the hydrolysis reaction of Microcrystalline Cellulose in the mixture obtained to step (1); By the suspension centrifugal 20min under 11000r/min obtained, then by the solid deionized water wash of centrifugal gained for several times, the pH value of the clear liquid obtained until centrifugal is 7; By the solid dry 8h at 105 DEG C cleaned, namely obtain the crystalline cellulose N2 that receives of 33.08g, productive rate is 82.7%.Measuring product by transmission electron microscope (TEM), to receive the median size of crystalline cellulose be 558nm, and crystalline cellulose of receiving is bar-shaped.
Preparation example 3
(1) 40g Microcrystalline Cellulose (purchased from Hubei Zhong Liao Chemical Co., Ltd., the median size of particle is 50 μm) being added concentration is in the 700mL aqueous sulfuric acid of 64 % by weight, and with the rotating speed high-speed stirring 3h of 250 turns/min at 45 DEG C;
(2) 3L deionized water is added to stop the hydrolysis reaction of Microcrystalline Cellulose in the mixture obtained to step (1); By the suspension centrifugal 15min under 11000r/min obtained, then by the solid deionized water wash of centrifugal gained for several times, the pH value of the clear liquid obtained until centrifugal is 7; By the solid dry 8h at 105 DEG C cleaned, namely obtain the crystalline cellulose N3 that receives of 33.96g, productive rate is 84.9%.Measuring product by transmission electron microscope (TEM), to receive the median size of crystalline cellulose be 370nm, and crystalline cellulose of receiving is bar-shaped.
Preparation example 4
(1) 40g Microcrystalline Cellulose (purchased from Hubei Zhong Liao Chemical Co., Ltd., the median size of particle is 50 μm) being added concentration is in the 700mL aqueous sulfuric acid of 64 % by weight, and with the rotating speed high-speed stirring 3h of 250 turns/min at 55 DEG C;
(2) 3L deionized water is added to stop the hydrolysis reaction of Microcrystalline Cellulose in the mixture obtained to step (1); By the suspension centrifugal 18min under 11000r/min obtained, then by the solid deionized water wash of centrifugal gained for several times, the pH value of the clear liquid obtained until centrifugal is 7; By the solid dry 12h at 105 DEG C cleaned, namely obtain the crystalline cellulose N4 that receives of 35.4g, productive rate is 88.5%.Measuring product by transmission electron microscope (TEM), to receive the median size of crystalline cellulose be 315nm, and crystalline cellulose of receiving is bar-shaped.
Preparation example 5
(1) 40g Microcrystalline Cellulose (purchased from Hubei Zhong Liao Chemical Co., Ltd., the median size of particle is 50 μm) being added concentration is in the 700mL aqueous sulfuric acid of 64 % by weight, and with the rotating speed high-speed stirring 7h of 150 turns/min at 55 DEG C;
(2) 3L deionized water is added to stop the hydrolysis reaction of Microcrystalline Cellulose in the mixture obtained to step (1); By the suspension centrifugal 15min under 11000r/min obtained, then by the solid deionized water wash of centrifugal gained for several times, the pH value of the clear liquid obtained until centrifugal is 7; By the solid dry 12h at 105 DEG C cleaned, namely obtain the crystalline cellulose N5 that receives of 36.6g, productive rate is 91.5%.Measuring product by transmission electron microscope (TEM), to receive the median size of crystalline cellulose be 185nm, and crystalline cellulose of receiving is bar-shaped.
Preparation example 6
(1) 40g Microcrystalline Cellulose (purchased from Hubei Zhong Liao Chemical Co., Ltd., the median size of particle is 50 μm) being added concentration is in the 860mL aqueous sulfuric acid of 50 % by weight, and with the rotating speed high-speed stirring 5h of 300 turns/min at 40 DEG C;
(2) 2.4L deionized water is added to stop the hydrolysis reaction of Microcrystalline Cellulose in the mixture obtained to step (1); By the suspension centrifugal 10min under 8000r/min obtained, then by the solid deionized water wash of centrifugal gained for several times, the pH value of the clear liquid obtained until centrifugal is 7; By the solid dry 8h at 110 DEG C cleaned, namely obtain the crystalline cellulose N6 that receives of 35.4g, productive rate is 88.5%.Measuring product by transmission electron microscope (TEM), to receive the median size of crystalline cellulose be 310nm, and crystalline cellulose of receiving is bar-shaped.
Preparation example 7
(1) 40g Microcrystalline Cellulose (purchased from Hubei Zhong Liao Chemical Co., Ltd., the median size of particle is 20 μm) being added concentration is in the 500mL aqueous sulfuric acid of 70 % by weight, and with the rotating speed high-speed stirring 9h of 150 turns/min at 55 DEG C;
(2) 1.6L deionized water is added to stop the hydrolysis reaction of Microcrystalline Cellulose in the mixture obtained to step (1); By the suspension centrifugal 15min under 6000r/min obtained, then by the solid deionized water wash of centrifugal gained for several times, the pH value of the clear liquid obtained until centrifugal is 7; By the solid dry 10h at 100 DEG C cleaned, namely obtain the crystalline cellulose N7 that receives of 34.88g, productive rate is 87.2%.Measuring product by transmission electron microscope (TEM), to receive the median size of crystalline cellulose be 280nm, and crystalline cellulose of receiving is bar-shaped.
Embodiment 1-7 is for illustration of the filtrate reducing effect of crystalline cellulose in drilling fluid of receiving provided by the invention.
Embodiment 1-7
The filter loss of crystalline cellulose in drilling fluid of receiving provided by the invention is measured according to the method in GB/T16783.1-2006.Concrete operations are:
(1) base slurry is configured: in 500mL tap water, add 20g sodium bentonite (purchased from Weifang Hua Wei wilkinite Group Plc) and 1g anhydrous sodium carbonate, airtight standing 24h stir 30min under 11000rpm rotating speed after, obtains the fresh water-based slurry that bentonite content is 4 % by weight.
(2) the above-mentioned fresh water-based slurry solution getting 400mL is put into ZNS-2 type and is pressed filter press (purchased from Qingdao Hong Xiang petroleum machinery Manufacturing Co., Ltd), measures its filter loss under 0.7MPa pressure in 30min, is the filter loss of fresh water-based slurry.
(3) in the above-mentioned fresh water-based slurry of 400mL, add the crystalline cellulose N1 that receives that 2g preparation example 1 obtains, after stirring, put into ZNS-2 type and press filter press, measure its filter loss under 0.7MPa pressure in 30min, what namely obtain that preparation example 1 obtains receives the filter loss of crystalline cellulose N1 in fresh water-based slurry;
The obtained filter loss of crystalline cellulose N2-N7 in fresh water-based slurry of receiving is measured in preparation example 2-7 respectively according to above method.The experimental result recorded is listed in Table 1.
Comparative example 1
Adopt the method identical with embodiment 1 to prepare fresh water-based to starch, unlike, in step (3), adopt the graphene oxide (DN1) (purchased from Nanjing Ji Cang company limited, median size is 210nm) of identical weight to replace receiving crystalline cellulose N1.The experimental result recorded is listed in Table 1.
Table 1
| Sample | FL/mL |
| Fresh water-based is starched | 27 |
| Fresh water-based slurry+N1 | 10.4 |
| Fresh water-based slurry+N2 | 21.4 |
| Fresh water-based slurry+N3 | 18.0 |
| Fresh water-based slurry+N4 | 14.8 |
| Fresh water-based slurry+N5 | 7.2 |
| Fresh water-based slurry+N6 | 13.1 |
| Fresh water-based slurry+N7 | 11.8 |
| Fresh water-based slurry+DN1 | 25.1 |
As can be seen from the result of table 1, provided by the invention there is specific dimensions receive crystalline cellulose as fluid loss additive for boring fluid, there is excellent filtrate loss controllability.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each the concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode.In order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (5)
1. Repone K-polyglycol drilling fluid, this drilling fluid contains fluid loss agent, it is characterized in that, described fluid loss agent is for receiving crystalline cellulose; The described median size receiving crystalline cellulose is 150-320nm; Described polymeric alcohol is one or more in polyoxyethylene glycol, polypropylene glycol, ethylene glycol/propylene glycol copolymers, polyglycerol and polyethylene glycol; Wherein, relative to the described drilling fluid of 100 weight parts, the content of described fluid loss agent is 0.1-5 weight part; Described drilling fluid is also containing soil with slurry, alkaline carbonate, inhibitor, tackifier, viscosity-depression agent, weighting agent, coating agent and lubricant; Wherein, relative to the described drilling fluid of 100 weight parts, the content of described soil with slurry is 2-4 weight part, the content of described alkaline carbonate is 0.1-1 weight part, and the content of described inhibitor is 0.2-3 weight part, and the content of described tackifier is 0.2-1 weight part, the content of described viscosity-depression agent is 0.2-1 weight part, the content of described weighting agent is 0.2-3 weight part, and the content of described coating agent is 0.2-1 weight part, and the content of described lubricant is 0.1-2 weight part; Wherein, described soil with slurry is wilkinite; Described inhibitor is one or more in small cation inhibitor and polyether diamine; Described tackifier are one or more in xanthan gum natural gum, xanthan gum, carboxymethyl starch, Walocel MT 20.000PV, Natvosol, carboxymethyl cellulose and Polyanionic Cellulose; Described viscosity-depression agent is one or more in feero-chromo-lignosulfonate, sodium polyacrylate, methyl silicon sodium alcoholate and Sulfonated Copolymer of Styrene and Maleic Anhydride; Described coating agent is one or more in partially hydrolyzed polyacrylamide, cationic polyacrylamide and polymerize aluminum chloride; Described lubricant is one or more in nonionogenic tenside and graphite.
2. a silicone drilling fluid, this drilling fluid contains fluid loss agent, it is characterized in that, described fluid loss agent is for receiving crystalline cellulose; The described median size receiving crystalline cellulose is 150-320nm; Organosilicon in described silicone drilling fluid be selected from methyl silicon sodium alcoholate, methyl silanol potassium and organic silicone potassium humate one or more; Wherein, relative to the described drilling fluid of 100 weight parts, the content of described fluid loss agent is 0.1-5 weight part; Described drilling fluid is also containing soil with slurry, alkaline carbonate, inhibitor, tackifier, viscosity-depression agent, weighting agent, coating agent and lubricant; Wherein, relative to the described drilling fluid of 100 weight parts, the content of described soil with slurry is 2-4 weight part, the content of described alkaline carbonate is 0.1-1 weight part, and the content of described inhibitor is 0.2-3 weight part, and the content of described tackifier is 0.2-1 weight part, the content of described viscosity-depression agent is 0.2-1 weight part, the content of described weighting agent is 0.2-3 weight part, and the content of described coating agent is 0.2-1 weight part, and the content of described lubricant is 0.1-2 weight part; Wherein, described soil with slurry is wilkinite; Described inhibitor is one or more in Repone K, small cation inhibitor and polyether diamine; Described tackifier are one or more in xanthan gum natural gum, xanthan gum, carboxymethyl starch, Walocel MT 20.000PV, Natvosol, carboxymethyl cellulose and Polyanionic Cellulose; Described viscosity-depression agent is one or more in feero-chromo-lignosulfonate, sodium polyacrylate and Sulfonated Copolymer of Styrene and Maleic Anhydride; Described coating agent is one or more in partially hydrolyzed polyacrylamide, cationic polyacrylamide and polymerize aluminum chloride; Described lubricant is one or more in nonionogenic tenside and graphite.
3. a cationic drilling fluid, this drilling fluid contains fluid loss agent, it is characterized in that, described fluid loss agent is for receiving crystalline cellulose; The described median size receiving crystalline cellulose is 150-320nm; Positively charged ion in described cationic drilling fluid is 2,3-epoxypropyltrimethylchloride chloride and/or 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride; Wherein, relative to the described drilling fluid of 100 weight parts, the content of described fluid loss agent is 0.1-5 weight part; Described drilling fluid is also containing soil with slurry, alkaline carbonate, inhibitor, tackifier, viscosity-depression agent, weighting agent, coating agent and lubricant; Wherein, relative to the described drilling fluid of 100 weight parts, the content of described soil with slurry is 2-4 weight part, the content of described alkaline carbonate is 0.1-1 weight part, and the content of described inhibitor is 0.2-3 weight part, and the content of described tackifier is 0.2-1 weight part, the content of described viscosity-depression agent is 0.2-1 weight part, the content of described weighting agent is 0.2-3 weight part, and the content of described coating agent is 0.2-1 weight part, and the content of described lubricant is 0.1-2 weight part; Wherein, described soil with slurry is wilkinite; Described inhibitor is Repone K and/or polyether diamine; Described tackifier are one or more in xanthan gum natural gum, xanthan gum, carboxymethyl starch, Walocel MT 20.000PV, Natvosol, carboxymethyl cellulose and polyanion; Described viscosity-depression agent is one or more in feero-chromo-lignosulfonate, sodium polyacrylate, methyl silicon sodium alcoholate and Sulfonated Copolymer of Styrene and Maleic Anhydride; Described coating agent is one or more in partially hydrolyzed polyacrylamide, cationic polyacrylamide and polymerize aluminum chloride; Described lubricant is one or more in nonionogenic tenside and graphite.
4. crystalline cellulose of receiving according to the drilling fluid in claim 1-3 described in any one, wherein, is bar-shaped.
5., according to the drilling fluid in claim 1-3 described in any one, wherein, relative to the described drilling fluid of 100 weight parts, the content of described fluid loss agent is 0.2-1 weight part.
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| CN107955586A (en) * | 2017-11-08 | 2018-04-24 | 中石化石油工程技术服务有限公司 | The cellulose nano-fibrous application as drilling fluid flow pattern regulator |
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| CN113046039B (en) * | 2021-05-20 | 2022-05-17 | 山东红锦石油技术开发有限公司 | High-temperature-resistant composite filtrate reducer for seawater drilling fluid and preparation method thereof |
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| US20130274149A1 (en) * | 2012-04-13 | 2013-10-17 | Schlumberger Technology Corporation | Fluids and methods including nanocellulose |
| CN103360616B (en) * | 2013-07-10 | 2015-12-02 | 武汉纺织大学 | A kind of film through graphene/nano crystalline cellulose dispersion liquid prepares the method for hybridized film |
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| CN107955586A (en) * | 2017-11-08 | 2018-04-24 | 中石化石油工程技术服务有限公司 | The cellulose nano-fibrous application as drilling fluid flow pattern regulator |
| CN107955586B (en) * | 2017-11-08 | 2021-03-02 | 中石化石油工程技术服务有限公司 | Application of cellulose nanofiber as flow pattern regulator for drilling fluid |
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