CN115340121A - Method for separating barite from shale gas drilling mud - Google Patents

Method for separating barite from shale gas drilling mud Download PDF

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Publication number
CN115340121A
CN115340121A CN202211258623.XA CN202211258623A CN115340121A CN 115340121 A CN115340121 A CN 115340121A CN 202211258623 A CN202211258623 A CN 202211258623A CN 115340121 A CN115340121 A CN 115340121A
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barite
slurry
drilling mud
shale gas
gas drilling
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彭青松
李乐军
王攀
罗培强
罗红莹
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Sichuan Junhe Environmental Protection Co ltd
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Sichuan Junhe Environmental Protection Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/46Sulfates
    • C01F11/462Sulfates of Sr or Ba
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03BSEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B9/00General arrangement of separating plant, e.g. flow sheets
    • B03B9/06General arrangement of separating plant, e.g. flow sheets specially adapted for refuse

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The invention discloses a method for separating barite from shale gas drilling mud, which comprises the steps of mixing dry shale gas drilling mud obtained after water and petroleum hydrocarbon are removed by a harmless treatment method with water to obtain slurry, adding dilute sulfuric acid into the slurry to disperse agglomerated dry slag particles, then screening the slurry by using screening equipment to obtain undersize slurry and oversize particles, and reselecting the undersize slurry by using reselection equipment to obtain barite concentrate and detritus tailings. The method takes the dry slag after harmless treatment as a separation object, and the residual product after barite extraction has no environmental hazard, can be used as a cement admixture and a fired ceramsite raw material, and improves the application and value of the dry slag; the barite is separated by a gravity separation method by utilizing the density difference between the barite and other components, the purity of the extracted barite is high, the barite reaches the industrial grade, the recycling of the barite is realized, and the mining requirement on the barite ore is relieved.

Description

Method for separating barite from shale gas drilling mud
Technical Field
The invention relates to the technical field of drilling waste treatment, in particular to a method for separating barite from shale gas drilling mud.
Background
In the well drilling of shale gas exploration and development, a weighting agent is one of indispensable important materials in a drilling fluid, and the weighting agent commonly used at present is barite. Barite is a non-renewable non-metallic mineral product, and the exploitation of barite ore has great damage to the environment, and based on the reasons of environmental protection and the like, the exploitation of barite ore is strictly limited in China at present. The annual consumption of barite in China is about 120-130 ten thousand tons, wherein the consumption of barite in the drilling industry is 70-80 ten thousand tons, and the barite is mainly used as a drilling weighting agent.
In the exploration and development of shale gas, after barite is used as a drilling weighting agent and added into drilling fluid, rock debris particles are carried to form drilling mud, and because chemical components, heavy metal ions and the like in the drilling mud have great pollution to the environment, the drilling mud needs to be subjected to harmless treatment. At present, the technology of harmless treatment of drilling mud is mature, the technology comprises a mud solid-liquid separation technology, a chemical additive solidification treatment drilling mud and the like, and dry shale gas drilling mud residues subjected to the harmless treatment contain weighting agent barite. At present, the content of barite in the harmless-treated drilling mud dry slag exceeds the limit of a cement additive, so that the drilling mud dry slag is difficult to be used as the cement additive for comprehensive utilization of resources, and if the drilling mud dry slag is recycled as a barite product, the grade cannot meet the requirement, so that the drilling mud dry slag is generally discarded as solid waste at present, and the barite contained in the drilling mud dry slag is lost in vain, so that the waste of the barite mineral resources is caused.
The technical personnel in the field are constantly working on how to separate the barite from the drilling mud to realize the recycling of the barite, and the main waste drilling fluid recycling method researched at home and abroad at present comprises the separation and recycling of the barite, drill cuttings and the like in the waste drilling mud. Wherein the barite is used to reformulate the drilling mud and the drill cuttings are used as a cement feedstock or directly as a building material. The barite recovery method which is disclosed at home and abroad at present is mainly a centrifugal sedimentation process. The process has the problems of high operation cost and incomplete separation, and because of the possibility of low-density large-particle barite and high-density small-particle barite, the mass difference between the two is very small, and the separation cannot be realized by a centrifugal technology. Centrifuge needs multistage progressively to improve the barite purity, the technology is complicated, patent CN101050695A discloses a system for recovering and aggravating the barite in the drilling fluid and removing useless solid phase, through the system of a set of organic connection, with two centrifuge series-connected together, divide two steps to handle the drilling fluid, solved the high-efficient separation of barite among the aggravating drilling fluid processing simultaneously, the dispersion is retrieved to the barite, prevent that the barite from deposiing, improve and aggravate drilling fluid treatment effeciency scheduling problem, when retrieving most barite, most detritus granule has been arranged, the consumption of barite has significantly reduced, the cost has been practiced thrift both, the environment has also been protected.
The patent CN 104609455A discloses a method for recovering barite from waste drilling mud, which utilizes a flotation separation method to separate the barite aiming at the characteristic that the waste drilling mud has a large amount of drill cutting powder and high content of soluble salt, improves the flotation efficiency by adjusting the pH value in waste liquid and optimizing a flotation additive, and the barite obtained by flotation can be used for preparing the drilling mud again through surface modification.
Disclosure of Invention
In view of the problems in the background art, the present application aims to provide a method for separating barite from shale gas drilling mud, so as to realize resource utilization of shale gas drilling mud.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a method of separating barite from shale gas drilling mud comprising the steps of:
A. removing water and petroleum hydrocarbon from the shale gas drilling mud by a harmless treatment method to obtain dry residue;
B. mixing the dry residue with water to prepare slurry, and adding dilute sulfuric acid into the slurry to adjust the pH of the slurry to 8-11;
C. b, screening the slurry obtained in the step B by using screening equipment to obtain undersize slurry and oversize particles, wherein the content of barite in the oversize particles is less than 3%;
D. and (4) reselecting the undersize slurry by using reselection equipment to obtain barite concentrate and rock debris tailings.
Further, the mass concentration of the slurry is 10-30%. The slurry with the concentration is convenient to mix and stir, and the pH value is easy to adjust.
Further, the mass percentage concentration of the dilute sulfuric acid is less than or equal to 70 percent. The dilute sulfuric acid used in the application is used for adjusting the pH value of slurry by utilizing the acidity of the dilute sulfuric acid, and the sulfuric acid with the mass percentage concentration higher than 70% mainly represents oxidation rather than acidity.
Further, the mesh number of the screen in the screening device is 325 meshes. According to the fact that the fineness of weighting agent barite powder used at present is 325 meshes, a 325-mesh screen is selected for screening slurry, primary separation can be conducted on barite and coarse particles, and meanwhile the content of barite in the coarse particles is less than 3%. The screening equipment is a linear vibrating screen or a disc vibrating screen.
Further, the gravity separation device selects a blanket machine or a shaker for gravity separation operation due to the particle size of the undersize slurry being smaller than 325 mesh.
Further, the oversize particles and the rock debris tailings are subjected to filter pressing dehydration treatment to obtain a rock debris filter cake with the water content of less than 30%, and the rock debris filter cake can be used as a cement admixture, a fired ceramsite raw material and the like due to separation of barite.
Further, the barite concentrate is subjected to filter pressing dehydration treatment to obtain a barite filter cake with the water content of less than 30%, the barite filter cake is dried to obtain a barite product, and the barite product can be used as a weighting agent.
The harmless treatment technology of the drilling mud is a mature treatment technology in the prior art, ions harmful to the environment are removed from the drilling mud through the harmless treatment, and residual dry slag is obtained through the recycling of oil products. The technical personnel in the field carry out the removal treatment of water and petroleum hydrocarbon on shale gas drilling mud according to the existing harmless treatment method to realize the oil recovery, and the obtained residual dry slag mainly comprises barite, detritus and a small amount of calcium hydroxide. Because the barite granule can form the agglomerate with other components in the dry sediment, can not directly separate the barite in the dry sediment, consequently this application adds water and prepares into the slurry with the dry sediment, and through adding the dilute sulfuric acid of dispersant and dissociating the agglomerate into monomer granule, then realizes the separation of barite and other components of detritus through screening and gravity separation. The dispersant dilute sulfuric acid can neutralize a small amount of calcium hydroxide in the dry slag, so that the dry slag is prevented from agglomerating due to the existence of the calcium hydroxide; meanwhile, the pH value of the slurry is adjusted by the dilute sulfuric acid serving as the dispersing agent, so that the surfaces of the dry slag particles are charged in the same way, and the dry slag particles are difficult to agglomerate according to the principle that like charges repel each other, thereby achieving the effect of dissociating the dry slag particles into monomer particles. The gravity separation method is a method for separating components according to the specific gravity difference of the components, is less influenced by the particle size, can realize the separation between the barite with large specific gravity and other components with small specific gravity, and has high purity of the barite separated by gravity separation.
Compared with the prior art, the invention has the following beneficial effects:
(1) The method takes the dry slag after harmless treatment as a separation object, and the residual product after barite extraction has no environmental hazard, can be used as a cement admixture and a fired ceramsite raw material, and improves the application and value of the dry slag;
(2) According to the method, the barite is separated by a gravity separation method by utilizing the density difference between the barite and other components, the purity of the extracted barite is high and reaches the industrial grade, the barite can be returned to a drilling platform to be used as a weighting agent for continuous use, the recycling of the barite is realized, and the mining requirement on the barite ore is relieved;
(3) The barite is extracted by physical separation, and only the dispersant dilute sulfuric acid is added into slurry to break up dry slag particles, so that secondary pollutants are not generated;
(4) The equipment technology related to the method is mature and reliable, and the method has the advantages of simple implementation, wide applicability and remarkable benefit.
Drawings
Fig. 1 is a schematic flow chart of the method of embodiments 1 to 3 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the following specific embodiments and accompanying drawings.
The dry slag treated by the drilling mud used in the following examples is the residual dry slag generated after the drilling mud generated in the shale gas exploitation place in Yibingwen county, sichuan is treated by a harmless treatment production line of the drilling mud of Chikawa peak science and technology development Limited company, the water and the petroleum hydrocarbon are removed, and the main components of the residual dry slag are as follows:
Figure 890861DEST_PATH_IMAGE001
the parameters of the used equipment models are as follows:
Figure 139440DEST_PATH_IMAGE002
the method for detecting the content of barite in the rock debris filter cake comprises the following steps: refer to the column labeled "JCT 1021.7-2007 chemical analysis of barite ore".
The method for detecting the components in the barite product comprises the following steps: refer to the Roche notation "JCT 1021.7-2007 chemical analysis method of barite ore".
The following examples 1 to 3 were carried out with reference to the process flow diagram shown in FIG. 1.
Example 1:
10kg of dry slag treated by drilling mud is taken, water is added and mixed to prepare slurry with the mass concentration of 10%, 50% of dilute sulfuric acid is added into the slurry to adjust the pH value of the slurry to be 8, then a disc vibrating screen (with the mesh number of 325 meshes) is used for screening the slurry to obtain oversize particles and undersize slurry, the undersize slurry is reselected by a table concentrator to obtain barite concentrate and rock debris tailings, the oversize particles and the rock debris tailings are dehydrated by a filter press to obtain rock debris filter cakes with the water content of less than 30%, the barite concentrate is dehydrated by the filter press and then dried by a dryer to obtain 3.35kg of barite products, and the recovery rate is 94%.
Through detection, the content of barite in the rock debris filter cake is 2.8%, and the rock debris filter cake can be used as a cement admixture and a fired ceramsite raw material.
The grade of the barite product is 87%, the granularity is smaller than 325 meshes, the water-soluble alkaline earth metal is 12mg/kg, the 75-micron screen residue is 1.7%, the viscosity effect is smaller than 46mPa & s, and the barite product meets the weighting agent parameter requirements specified in GB/T5005-2010 drilling fluid material Specification.
Example 2:
10kg of drilling mud disposal dry slag is mixed with water to prepare slurry with the mass concentration of 30%, 50% of dilute sulfuric acid is added into the slurry to adjust the pH value of the slurry to be 11, then a linear vibrating screen (the mesh number of the screen is 325 meshes) is used for screening the slurry to obtain oversize particles and undersize slurry, the undersize slurry is reselected by a blanket machine to obtain barite concentrate and rock debris tailings, the oversize particles and the rock debris tailings are dehydrated by a filter press to obtain rock debris filter cakes with the water content of less than 30%, the barite concentrate is dehydrated by the filter press and then dried by a dryer to obtain 3.14kg of barite products, and the recovery rate is 86%.
The detection shows that the content of barite in the rock debris filter cake is 6.3 percent, and the rock debris filter cake can be used as a cement admixture and a firing ceramsite raw material.
The grade of the barite product is 85%, the granularity is smaller than 325 meshes, the water-soluble alkaline earth metal is 12mg/kg, the 75-micron screen residue is 1.7%, the viscosity effect is smaller than 46mPa & s, and the barite product meets the weighting agent parameter requirements specified in GB/T5005-2010 drilling fluid material Specification.
Example 3:
10kg of drilling mud disposal dry slag is taken and mixed with water to prepare slurry with the mass concentration of 20%, 50% dilute sulfuric acid is added into the slurry to adjust the pH value of the slurry to 9.5, then a disc vibration sieve (with the mesh number of 325 meshes) is used for sieving the slurry to obtain oversize particles and undersize slurry, the undersize slurry is reselected by a table concentrator to obtain barite concentrate and rock debris tailings, the oversize particles and the rock debris tailings are dehydrated by a filter press to obtain rock debris filter cake with the water content of less than 30%, the barite concentrate is dehydrated by the filter press and then dried by a dryer to obtain 3.24kg of barite product, and the recovery rate is 91%.
Through detection, the barite content in the rock debris filter cake is 4.1%, and the rock debris filter cake can be used as a cement admixture and a fired ceramsite raw material.
The grade of the barite product is 87%, the granularity is smaller than 325 meshes, the water-soluble alkaline earth metal is 12mg/kg, the 75-micron screen residue is 1.7%, the viscosity effect is smaller than 46mPa & s, and the barite product meets the weighting agent parameter requirements specified in GB/T5005-2010 drilling fluid material Specification.
Comparative example 1:
10kg of drilling mud treated dry slag is mixed with water to prepare slurry with the mass concentration of 10%, 50% of sulfurous acid is added into the slurry to adjust the pH value of the slurry to be 8, then a disc vibrating screen (with the mesh number of 325 meshes) is used for screening the slurry to obtain oversize particles and undersize slurry, the undersize slurry is reselected by a table concentrator to obtain barite concentrate and rock debris tailings, the oversize particles and the rock debris tailings are dehydrated by a filter press to obtain rock debris filter cakes with the water content of less than 30%, the barite concentrate is dehydrated by the filter press and then dried by a dryer to obtain 2.83kg of barite products, the recovery rate is 74%, and the loss rate of barite is high.
The detection shows that the content of barite in the rock debris filter cake is 11.2 percent, and the barite content is too high, so the rock debris filter cake is not suitable to be used as a cement admixture and a raw material for firing ceramsite.
The grade of the barite product is 81 percent, and the parameter requirement of the weighting agent specified in GB/T5005-2010 drilling fluid material Specification cannot be met.
Comparative example 2:
10kg of dry slag treated by drilling mud is mixed with water to prepare slurry with the mass concentration of 10%, 50% formic acid water solution is added into the slurry to adjust the pH value of the slurry to be 8, then a disc vibrating screen (with the mesh number of 325 meshes) is used for screening the slurry to obtain oversize particles and undersize slurry, the undersize slurry is reselected by a table concentrator to obtain barite concentrate and rock debris tailings, the oversize particles and the rock debris tailings are dehydrated by a filter press to obtain rock debris filter cake with the water content of less than 30%, the barite concentrate is dehydrated by the filter press and then dried by a dryer to obtain 2.63kg of barite product, the recovery rate is 67%, and the loss rate of the barite is high.
The detection shows that the content of barite in the rock debris filter cake is 13.9 percent, and the barite content is too high, so the rock debris filter cake is not suitable to be used as a cement admixture and a raw material for firing ceramsite.
The grade of the barite product is 79 percent, and the barite product cannot meet the weighting agent parameter requirement specified in GB/T5005-2010 drilling fluid material Specification.
Comparative example 3:
10kg of dry slag of drilling mud treatment is taken, water is added and mixed to prepare slurry with the mass concentration of 10%, then a disc vibrating screen (with the mesh number of 325 meshes) is used for screening the slurry to obtain oversize particles and undersize slurry, the undersize slurry is reselected by a table concentrator to obtain barite concentrate and detritus tailings, the oversize particles and the detritus tailings are dehydrated by a filter press to obtain detritus filter cakes with the water content of less than 30%, the barite concentrate is dehydrated by the filter press and then dried by a dryer to obtain 2.37kg of barite products, the recovery rate is 58%, and the loss rate of barite is high.
The detection shows that the content of barite in the rock debris filter cake is 17 percent, and the content of barite is too high, so that the rock debris filter cake is not suitable to be used as a cement admixture and a raw material for firing ceramsite.
The grade of the barite product is 76 percent, and the barite product cannot meet the weighting agent parameter requirement specified in GB/T5005-2010 drilling fluid material Specification.
Comparative example 4:
10kg of dry slag treated by drilling mud is mixed with water to prepare slurry with the mass concentration of 10%, 50% of dilute sulfuric acid is added into the slurry to adjust the pH value of the slurry to be 8, then a disc vibrating screen (with the mesh number of 325 meshes) is used for screening the slurry to obtain oversize particles and undersize slurry, the undersize slurry is separated by a centrifugal separator to obtain barite concentrate and rock debris tailings, the oversize particles and the rock debris tailings are dehydrated by a filter press to obtain rock debris filter cakes with the water content of less than 30%, the barite concentrate is dehydrated by the filter press and then dried by a dryer to obtain 2.99kg of barite products, the recovery rate is 82%, and the loss rate of the barite is higher.
Through detection, the content of barite in the rock debris filter cake is 7.96 percent, and the barite content is too high, so that the rock debris filter cake is not suitable for being used as a cement admixture and a raw material for firing ceramsite.
The grade of the barite product is 85%, the granularity is smaller than 325 meshes, the water-soluble alkaline earth metal is 12mg/kg, the 75-micron surplus is 1.7%, and the viscosity effect is smaller than 46mPa & s, so that the barite product meets the weighting agent parameter requirements specified in GB/T5005-2010 drilling fluid material Specification, but the grade is lower than that of the product in example 1, which indicates that the centrifugal separation cannot completely separate the barite concentrate from the rock debris tailings.
Comparative example 5:
the procedure is as in example 1 except that the pH of the slurry is adjusted to 7 or 12.
When the pH value of the slurry is 7, the detection results of the rock debris filter cake and the barite product are the same as those of the example 1; when the pH value of the slurry is 12, the content of the barite in the rock debris filter cake is 15.4%, and the grade of the barite product is 81%, which are not in accordance with the requirements. In the production process, the closer the pH is to 7, the greater the difficulty of controlling the pH by the production process is, so that the pH is controlled to be 8-11 by the method, and the requirement of the method can be met.
In conclusion, the method for separating barite from shale gas drilling mud provided by the invention can recover most of barite, reduce the content of barite in rock debris, recycle harmless treated dry slag and improve the utilization rate of shale gas drilling mud.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.

Claims (8)

1. A method of separating barite from shale gas drilling mud, the method comprising: the method comprises the following steps:
A. removing water and petroleum hydrocarbon from the shale gas drilling mud by a harmless treatment method to obtain dry residue;
B. mixing the dry residue with water to prepare slurry, and adding dilute sulfuric acid into the slurry to adjust the pH of the slurry to 8-11;
C. b, screening the slurry obtained in the step B by using screening equipment to obtain undersize slurry and oversize particles, wherein the content of barite in the oversize particles is less than 3%;
D. and (4) reselecting the undersize slurry by using reselection equipment to obtain barite concentrate and rock debris tailings.
2. The method of separating barite from shale gas drilling mud as claimed in claim 1, wherein: the mass concentration of the slurry is 10-30%.
3. The method of separating barite from shale gas drilling mud as claimed in claim 1, wherein: the mass percentage concentration of the dilute sulfuric acid is less than or equal to 70 percent.
4. The method of separating barite from shale gas drilling mud as claimed in claim 1, wherein: the mesh number of the screen in the screening equipment is 325 meshes.
5. The method of separating barite from shale gas drilling mud as claimed in claim 1, wherein: the screening equipment is a linear vibrating screen or a disc vibrating screen.
6. The method of separating barite from shale gas drilling mud as claimed in claim 1, wherein: the reselection device selects a blanket machine or a shaker.
7. The method of separating barite from shale gas drilling mud as claimed in claim 1, wherein: and carrying out filter pressing dehydration treatment on the oversize particles and the rock debris tailings.
8. The method of separating barite from shale gas drilling mud as claimed in claim 1, wherein: and carrying out filter pressing and dehydration treatment on the barite concentrate to obtain a barite filter cake, and drying the barite filter cake to obtain a barite product.
CN202211258623.XA 2022-10-14 2022-10-14 Method for separating barite from shale gas drilling mud Pending CN115340121A (en)

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Application publication date: 20221115