CN117050743B - Preparation process, system and control system of low-density epoxy resin fracturing propping agent - Google Patents
Preparation process, system and control system of low-density epoxy resin fracturing propping agent Download PDFInfo
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- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 description 2
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 2
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- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
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- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 2
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8362—Mixing plants; Combinations of mixers combining mixing with other treatments with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1862—Stationary reactors having moving elements inside placed in series
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
-
- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D27/00—Simultaneous control of variables covered by two or more of main groups G05D1/00 - G05D25/00
- G05D27/02—Simultaneous control of variables covered by two or more of main groups G05D1/00 - G05D25/00 characterised by the use of electric means
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Automation & Control Theory (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a preparation process, a system and a control system of a low-density epoxy resin fracturing propping agent, and belongs to the technical field of petroleum and natural gas exploitation and development. The preparation process comprises the steps of proportioning, pre-curing, heating, primary reaction, secondary reaction, tertiary reaction, post-curing and separation; also provided are a preparation system and a control system; finally, the epoxy resin fracturing propping agent meeting the development requirements of petroleum and natural gas exploitation is obtained, and the density is ensured to be less than or equal to 1.18g/cm 3 The roundness is more than or equal to 0.9, the sphericity is more than or equal to 0.9, the breakage resistance is less than or equal to 3%, the acid solubility is less than or equal to 0.2%, the size distribution range is 300-2000 mu m, the export of oil gas is facilitated, the return discharge amount is small, and the oil gas production efficiency is greatly improved. The preparation process, the preparation system and the control system are limited, so that the epoxy resin fracturing propping agent with excellent performance can be obtained; but also can ensure the stability, the order and the controllability of the preparation production line, and satisfy the following requirementsAnd the industrial mass production requirement.
Description
Technical Field
The invention relates to a preparation process, a system and a control system of a low-density epoxy resin fracturing propping agent, and belongs to the technical field of petroleum and natural gas exploitation and development.
Background
Hydraulic fracturing technology is a major measure to increase oil and gas production. In the petroleum exploitation process, after the high-closure-pressure low-permeability ore deposit is subjected to fracturing treatment, an oil and gas stratum is cracked, a fracturing propping agent enters the stratum along with high-pressure fracturing fluid and is filled in the cracks, and the fracturing propping agent mainly plays a role in supporting the cracks and preventing the cracks from being closed due to stress release, so that the stratum is promoted to maintain high diversion capacity, and the yield of petroleum and natural gas is increased. The fracturing propping agent plays an indispensable important role in the fracturing technology, and the problems of material selection, use, migration and the like of the fracturing propping agent have important influence on the exploitation efficiency of oil gas. At present, widely applied quartz sand mold propping agents and ceramsite propping agents respectively have the defects of low strength, high density and the like, and polymer fracturing fluid with environmental pollution is adopted. The fracturing propping agent with the advantages of high strength, low density and environmental protection is not found at home and abroad, so that the novel fracturing propping agent with low density, high strength, good temperature resistance and low construction difficulty is a trend of development.
Compared with the fracturing propping agent in the prior art, the fracturing propping agent is coated with resin, and the density of the fracturing propping agent can be partially reduced by using a small amount of epoxy resin with most phenolic resin, so that the fracture resistance is improved. But the coated proppants are more dense; in addition, in the technology, the aggregate is generally quartz sand or ceramic with higher density, so that the density of the fracturing propping agent is still higher, and a polymer viscous fracturing fluid is needed Pressing in and guiding out the steel plate can cause construction difficulty, and meanwhile, the steel plate is inconvenient to pump into the underground, such as: the prior art "CN105985767a proppants and methods of making the same. And, carbon Ceramics developed a low density ceramic proppant with a specific gravity of 2.55g/cm 3 The method is suitable for slickwater fracturing; saint Gobain also introduced Versalite series low density ceramsite proppants, which have low density and high strength characteristics, and can control density by adjusting pore size; the Preferred sand companies have recently developed proppant technology that aggregates bubbles, and after treating silica sand with a special surfactant by the FloPRO PTT technology, the silica sand can be suspended in water. In the related technical field in China, a recently reported Daqing enterprise uses a thermoplastic material (polystyrene) as a base material, and a granular propping agent is prepared through a granulating process, but the granular propping agent is poor in compression strength, temperature resistance, performance retention rate and long-term flow conductivity and cannot be used under medium-high closing pressure and higher temperature.
Furthermore, "low density proppant particles and their use" are disclosed in prior art CN101346324, employing composite proppant particles to improve the flow of a primary fluid through a support channel, wherein the composite particles comprise a plurality of high strength microbubbles and a resin binder; and, CN109321226a discloses "a preparation method of a fracturing propping agent", CN109321227a discloses "an epoxy resin fracturing propping agent", and CN112048294A discloses "an epoxy resin fracturing propping agent", but the following problems still exist: the related formula is in a laboratory stage, or the production efficiency of the related preparation method is low, the stability is poor, and the industrial production cannot be expanded, so that the related formula is limited to small tests or pilot tests; in addition, the adaptive automation control technology is still blank.
Disclosure of Invention
In order to overcome the defects in the prior art, the technical scheme provides a preparation process, a system and a control system of the low-density epoxy resin fracturing propping agent. In the technical proposal, not only provides a material with excellent performance (density is less than or equal to 1.18 g/cm) 3 The roundness is more than or equal to 0.9, the sphericity is more than or equal to 0.9, the breakage resistance rate is less than or equal to 3%, and the acid solubilityLess than or equal to 0.2 percent and the size distribution range is 300-2000 mu m), and a preparation process and a control system which are suitable for the epoxy resin fracturing propping agent are provided for the epoxy resin fracturing propping agent, and the stability, the order and the controllability of the production process are ensured, so that the industrial, automatic and economic mass production is satisfied.
In order to achieve the technical purpose, the following technical scheme is provided:
the first object of the present technical solution is to provide: the low-density epoxy resin fracturing propping agent comprises the following components in parts by mass:
100 parts of epoxy resin;
10-100 parts of curing agent;
0.1-10 parts of promoter;
1-30 parts of toughening agent;
0.1-10 parts of surface auxiliary agent;
200-2000 parts of inert medium;
the indexes of the epoxy resin fracturing propping agent comprise: the density is less than or equal to 1.18g/cm 3 The roundness is more than or equal to 0.9, the sphericity is more than or equal to 0.9, the breakage resistance is less than or equal to 3%, the acid solubility is less than or equal to 0.2%, and the size distribution range is 300-2000 mu m.
Further, the epoxy resin is one or a mixture of more than two of bisphenol A type epoxy resin E-51, bisphenol A type epoxy resin E-44, bisphenol A type epoxy resin E-20, bisphenol F type epoxy resin NPEF170, phenolic type epoxy resin F-44, phenolic type epoxy resin F-51 and multifunctional epoxy AG-80 and SK-0430. The epoxy resin is further limited, can better participate in a crosslinked network, provides excellent mechanical properties, and keeps the high breakage resistance of the epoxy resin propping agent.
Further, the curing agent is one or a mixture of more than two of modified hexamethylenediamine, dicyandiamide, modified imidazole, anhydride and phenolic resin. Further limitation of the curing agent can better cure raw material epoxy resin and provide a crosslinked network.
Further, the accelerator is one or a mixture of more than two of phenyldimethylurea, 2, 4-toluene dimethylurea, 2,4, 6-tris (dimethylaminomethyl) phenol, N-dimethylbenzylamine, triethanolamine, 2-methylimidazole and modified imidazole. The accelerator is further limited, so that the curing agent can better accelerate the curing of the raw material epoxy resin.
Further, the toughening agent is one or a mixture of more than two of polyether type toughening agent, polyurethane type toughening agent, polytetrahydrofuran toughening agent, nitrile rubber toughening agent and latent polyurethane toughening agent. The toughening agent is further limited, so that a tough crosslinked network can be better provided for the cured epoxy resin, and further, the performance index of the epoxy resin fracturing propping agent is ensured, so that the actual requirement is met.
Further, the surface auxiliary agent is one or the mixture of more than two of polyacrylic acid, organosilicon polymer, modified polyacrylic acid and modified organosilicon. The surface auxiliary agent is further limited, so that the epoxy resin mixed solution can be well assisted to be spherical and dispersed in an inert medium.
Further, the inert medium is one or a mixture of more than two of soybean oil, palm oil and methyl silicone oil (viscosity 1000-10000 mPa.s). The inert medium has poor compatibility with the raw material epoxy resin, is used as a reaction medium, further limits the inert medium, can better provide a product forming environment, and ensures that the epoxy resin dispersed into a sphere is solidified and formed into sphere particles.
The second object of the present technical solution is to provide: the preparation process of the fracturing propping agent suitable for the low-density epoxy resin comprises the following steps of:
s1, proportioning: respectively feeding epoxy resin, a curing agent, an accelerator, a toughening agent and a surface auxiliary agent into a batching tank, and stirring and mixing under the conditions of normal temperature and normal pressure to obtain a resin mixed solution;
wherein, the weight parts of epoxy resin, curing agent, accelerator, toughening agent and surface auxiliary agent are calculated as 100: 10-100: 0.1 to 10: 1-30: 0.1 to 10, control: the charging flow rates of the epoxy resin, the curing agent, the accelerator, the toughening agent and the surface auxiliary agent are respectively 450-550 cm 3 /min、450～550cm 3 /min、200～300cm 3 /min、100～200 cm 3 Per minute and 50-100 cm 3 Stirring at 30-100 r/min for 20-40 min;
s2, pre-curing: the cold inert medium in the inert medium storage tank is cooled to 120 cm to 140cm in flow rate 3 Introducing the mixture into a temporary storage tank for resin mixed solution in a minute, and then controlling the flow rate of the resin mixed solution in the material mixing tank to be 450-550 cm 3 Introducing the mixture into a temporary storage tank of the resin mixed solution in a minute, and controlling the content of the resin mixed solution in each liter of cold inert medium to be 0.05-0.5 kg, so as to disperse phases;
s3, heating: introducing cold inert medium into an inert medium heating tank, and heating at 100-150 ℃ and normal pressure to obtain hot inert medium;
wherein, set up electric heater: 380V of power supply, 28KW of thermal power;
s4, primary reaction: controlling the flow rate of the thermal inert medium to be 800-1200 cm 3 Introducing the mixture into a first-stage reaction kettle per minute, and controlling the flow rate of the disperse phase to be 100-200 cm after the temperature of the thermal inert medium in the first-stage reaction kettle is stabilized at 100-150 DEG C 3 Introducing/min into a first-stage reaction kettle, stirring at the temperature of 100-150 ℃ at the rotating speed of 80-120 r/min and the pressure of 0.08-0.12 MPa, and performing a first-stage reaction to obtain a first-stage reaction liquid with the size distribution range of 3-6 mm;
s5 secondary reaction: controlling the flow rate of the primary reaction liquid to be 180-220 cm 3 Introducing/min into a secondary reaction kettle, stirring at the temperature of 100-150 ℃ at the rotating speed of 80-120 r/min and the pressure of 0.08-0.12 MPa, and performing secondary reaction to obtain a secondary reaction solution with the size distribution range of 0.30-2 mm;
s6, three-stage reaction: controlling the flow rate of the secondary reaction liquid to be 230-270 cm 3 Introducing/min into a three-stage reaction kettle, stirring at the temperature of 100-150 ℃ and the rotating speed of 80-120 r/min, and carrying out three-stage reaction;
s7, post-curing: controlling the flow rate of the tertiary reaction liquid to be 120-180 cm 3 Introducing into a coil reactor at 100-150 deg.C and normal pressure for post-curing to obtain the final product；
S8, separation: controlling the flow rate of the product liquid which is completely solidified to be 180-220 cm 3 Introducing the epoxy resin into a separating cylinder for min, and filtering by a filter screen in the separating cylinder to obtain the epoxy resin fracturing propping agent;
wherein, the mesh number of the filter screen is 10-50 meshes, and the definition of the pore diameter of the filter screen is better matched with the size of the epoxy resin fracturing propping agent product.
Furthermore, the filtered inert medium is directly recycled to the inert medium heating tank to complete the continuous production process, so that on one hand, the recycling of the inert medium is realized, and on the other hand, the recycling of heat energy is realized, namely, the energy consumption of the electric heater is reduced, and the recycling economy and the environmental protection economy are realized.
The third object of the present technical solution is to provide: the preparation system suitable for the low-density epoxy resin fracturing propping agent comprises an epoxy resin storage tank, a curing agent storage tank, an accelerator storage tank, a toughening agent storage tank, a surface auxiliary agent storage tank, a batching tank, a resin mixed liquid temporary storage tank, a primary reaction kettle, a secondary reaction kettle, a tertiary reaction kettle, a coil pipe reactor and a separating barrel, wherein the epoxy resin storage tank is connected with the batching tank through an epoxy resin feeding pipe, the curing agent storage tank is connected with the batching tank through a curing agent feeding pipe, the accelerator storage tank is connected with the batching tank through an accelerator feeding pipe, the toughening agent storage tank is connected with the batching tank through a toughening agent feeding pipe, and the surface auxiliary agent storage tank is connected with the batching tank through a surface auxiliary agent feeding pipe;
the material outlet of the batching tank is connected with the material inlet of the resin mixed liquid temporary storage tank through a conveying pipe I, and the resin mixed liquid temporary storage tank is arranged at the rear side of a station of the batching tank; the feeding port of the resin mixed liquid temporary storage tank is also connected with a cold inert medium conveying pipe; the material outlet of the resin mixed solution temporary storage tank is connected with the material inlet of the first-stage reaction kettle through a conveying pipe II, the first-stage reaction kettle is arranged at the rear side of a station of the resin mixed solution temporary storage tank, and the first-stage reaction kettle is connected with a heat inert medium conveying pipe; the discharge port of the first-stage reaction kettle is connected with the feed port of the second-stage reaction kettle through a conveying pipe III, and the second-stage reaction kettle is arranged at the rear side of a station of the first-stage reaction kettle; the discharge port of the secondary reaction kettle is connected with the feed port of the tertiary reaction kettle through a conveying pipe IV, and the tertiary reaction kettle is arranged at the rear side of a station of the secondary reaction kettle; the discharge port of the three-stage reaction kettle is connected with the feed port of a coil pipe reactor through a conveying pipe V, and the coil pipe reactor is arranged at the rear side of a station of the three-stage reaction kettle; the discharge port of the coil pipe reactor is connected with the feed port of a separating cylinder through a conveying pipe VI, and the separating cylinder is arranged at the rear side of a station of the coil pipe reactor; the discharge port of the separating cylinder is connected with an epoxy resin fracturing propping agent temporary storage tank;
A continuous passage for preparing the epoxy resin fracturing propping agent is formed among the material mixing tank, the resin mixed liquid temporary storage tank, the primary reaction kettle, the secondary reaction kettle, the tertiary reaction kettle, the coil pipe reactor and the separating cylinder;
wherein, batching jar: the inside of the device is provided with a frame stirrer which is connected with a vertical gear reducer and a frequency converter, the top of the device is provided with an epoxy resin feed inlet, a curing agent feed inlet, an accelerator feed inlet, a toughening agent feed inlet, a surface auxiliary agent feed inlet, a standby port and an exhaust port, the middle part of the device is provided with a sight glass port, and the lower part of the device is provided with a discharge port;
resin mixed liquid temporary storage tank: the feeding port of the resin mixed liquid temporary storage tank is arranged at the top of the resin mixed liquid temporary storage tank, the top is also provided with a standby port, an emptying port and a cold inert medium inlet, and the bottom is provided with a disperse phase outlet;
first-stage reaction kettle: a frame stirrer is arranged in the inner part, and a transverse blade in the frame stirrer turns upwards clockwise at 45 degrees; the surface of the stirrer needs to be coated with a release agent; the frame type stirrer is connected with a vertical gear reducer and a frequency converter; the discharge port of the first-stage reaction kettle is arranged at the upper part of the first-stage reaction kettle, the middle part is provided with a sight glass port, and the lower part is provided with a disperse phase inlet, a thermal inert medium inlet and an emptying port;
And (3) a secondary reaction kettle: a frame stirrer is arranged in the inner part, and a transverse blade in the frame stirrer turns upwards clockwise at 45 degrees; the surface of the stirrer needs to be coated with a release agent; the frame type stirrer is connected with a vertical gear reducer and a frequency converter; the discharge port of the secondary reaction kettle is arranged at the upper part of the secondary reaction kettle, the top of the secondary reaction kettle is provided with a vent, and an internal thread ball valve is sleeved in the vent; the middle part is provided with a sight glass opening, and the lower part is provided with a first-stage reaction liquid inlet;
three-stage reaction kettle: a double-spiral belt stirrer is arranged in the inner part of the stirring tank, and the double-spiral belt turns upwards clockwise; the surface of the stirrer needs to be coated with a release agent; the double helical ribbon stirrer is connected with a vertical gear reducer and a frequency converter; the discharge port of the three-stage reaction kettle is arranged at the upper part of the three-stage reaction kettle, the top of the three-stage reaction kettle is provided with a vent, and an internal thread ball valve is sleeved in the vent; the lower part is provided with a secondary reaction liquid inlet;
coil reactor: the top is connected by a bolt through an integral movable cover; the heat insulating material is perlite or rock wool, the upper part is provided with a three-stage reaction liquid inlet, and the lower part is provided with a product liquid outlet.
Further, the resin mixed liquor temporary storage tank is connected with an inert medium storage tank through a cold inert medium conveying pipe, the inert medium storage tank is connected with an inert medium heating tank through an inert medium inlet pipe, and the inert medium heating tank is connected with the primary reaction kettle through a hot inert medium conveying pipe;
Wherein, inert medium storage tank: the top is connected by a half-open movable cover and a bolt; the upper part is provided with an overflow port, and the lower part is provided with a cold inert medium outlet;
an inert medium heating tank: the heat insulating material is perlite or rock wool, the upper part is provided with a cold inert medium inlet, a reflux port, a vent, an overflow port and a circulation port, and the lower part is provided with a hot inert medium outlet.
Further, an inert medium outlet on the separating cylinder is connected with a reflux port of the inert medium heating tank through a recovery pipe.
Further, at least two separating drums are arranged, a coil reactor discharge hole is connected with a first-stage separating drum feed inlet, a first-stage separating drum discharge hole is connected with a next-stage separating feed inlet, separating drums are sequentially connected, and a last-stage separating drum discharge hole is connected with an epoxy resin fracturing propping agent temporary storage tank. And the hierarchical filtration can be performed according to actual requirements.
The fourth object of the present technical solution is to provide: the control system suitable for the low-density epoxy resin fracturing propping agent is arranged in the epoxy resin fracturing propping agent preparation system and comprises a DCS controller, wherein the DCS controller is connected with a human-computer interface through a data input interface, is connected with a data acquisition unit through a data feedback interface and is connected with an execution unit through a data output interface;
The DCS controller comprises a batching control module, a pre-curing control module, a primary reaction control module, a secondary reaction control module, a tertiary reaction control module, a post-curing control module and a separation control module;
the data acquisition unit is arranged in the epoxy resin fracturing propping agent preparation system and comprises a sensor group for data acquisition and transmission in the epoxy resin fracturing propping agent preparation process;
the execution unit is arranged in the epoxy resin fracturing propping agent preparation system and comprises a device group for preparing and regulating the epoxy resin fracturing propping agent;
in addition, the DCS controller also comprises an inert medium heating control module, an alarm control module and a cleaning control module;
wherein, the DCS controller: on one hand, the information of a batching process and regulation thereof, the information of a pre-curing process and regulation thereof, the information of a primary reaction process and regulation thereof, the information of a secondary reaction process and regulation thereof, the information of a tertiary reaction process and regulation thereof, the information of a post-curing process and regulation thereof, the information of a separation process and regulation thereof, the information of an inert medium heating process and regulation thereof, the information of safety early warning information and the information of cleaning requirements are received from a human-computer interface, and on the other hand, the batching process information, the pre-curing process information, the information of the primary reaction process, the information of the secondary reaction process, the information of the tertiary reaction process, the information of the post-curing process, the information of the separation process, the information of the inert medium heating process, the information of safety early warning information and the information are received from a data acquisition unit, so that information analysis, comparison and judgment are completed; the execution unit sends out an instruction, and the data acquisition unit sends out a data acquisition instruction;
Human-machine interface: the method comprises the steps of finishing the input of a batching process and information of regulation and control thereof, a pre-curing process and information of regulation and control thereof, a primary reaction process and information of regulation and control thereof, a secondary reaction process and information of regulation and control thereof, a tertiary reaction process and information of regulation and control thereof, a post-curing process and information of regulation and control thereof, a separation process and information of regulation and control thereof, an inert medium heating process and information of regulation and control thereof, safety pre-warning information and cleaning requirement information. For the arrangement on the human-computer interface, a multifunctional table, a corresponding identification icon, a switch control key, a regulation control key and the like can be arranged;
a data acquisition unit: receiving a data acquisition instruction sent by a DCS controller, completing acquisition and transmission of a batching process and information of regulation and control thereof, a pre-curing process and information of regulation and control thereof, a primary reaction process and information of regulation and control thereof, a secondary reaction process and information of regulation and control thereof, a tertiary reaction process and information of regulation and control thereof, a post-curing process and information of regulation and control thereof, a separation process and information of regulation and control thereof, an inert medium heating process and information of regulation and control thereof, safety early warning information and cleaning requirement information, and feeding back to the DCS controller;
an execution unit: and completing the instruction sent by the DCS controller.
Further, the sensor group comprises an epoxy resin feeding flowmeter, a curing agent feeding flowmeter, an accelerator feeding flowmeter, a toughening agent feeding flowmeter and a surface auxiliary agent feeding flowmeter which are connected with the batching control module;
the device also comprises a resin mixed liquid feeding flowmeter and a cold inert medium feeding flowmeter I which are connected with the pre-curing control module;
the system also comprises a disperse phase feeding flowmeter, a thermal inert medium feeding flowmeter, a primary reaction kettle temperature sensor and a primary reaction kettle pressure sensor which are connected with the primary reaction control module;
the device also comprises a first-stage reaction liquid feeding flowmeter, a second-stage reaction kettle temperature sensor and a second-stage reaction kettle pressure sensor which are connected with the second-stage reaction control module;
the device also comprises a secondary reaction liquid feeding flowmeter, a tertiary reaction kettle temperature sensor and a tertiary reaction kettle pressure sensor which are connected with the tertiary reaction control module;
the device also comprises a three-stage reaction liquid feeding flowmeter, a coil reactor temperature sensor and a coil reactor pressure sensor which are connected with the post-curing control module;
the product liquid feeding flowmeter is connected with the separation control module;
the device also comprises a cold inert medium feeding flowmeter II and an inert medium heating tank temperature sensor which are connected with the inert medium heating control module.
Further, the equipment group comprises an epoxy resin storage tank, a curing agent storage tank, an accelerator storage tank, a toughening agent storage tank, a surface auxiliary agent storage tank, a material mixing tank, a resin mixed liquid temporary storage tank, a primary reaction kettle, a secondary reaction kettle, a tertiary reaction kettle, a coil reactor and a separation barrel;
the epoxy resin feeding flowmeter is arranged on an epoxy resin feeding pipe between the epoxy resin storage tank and the batching tank, the curing agent feeding flowmeter is arranged on a curing agent feeding pipe between the curing agent storage tank and the batching tank, the accelerator feeding flowmeter is arranged on an accelerator feeding pipe between the accelerator storage tank and the batching tank, the toughening agent feeding flowmeter is arranged on a toughening agent feeding pipe between the toughening agent storage tank and the batching tank, and the surface auxiliary agent feeding flowmeter is arranged on a surface auxiliary agent feeding pipe between the surface auxiliary agent storage tank and the batching tank;
the resin mixed liquid feeding flowmeter is arranged on a conveying pipe I between the batching tank and the resin mixed liquid temporary storage tank, and the cold inert medium feeding flowmeter I is arranged on a cold inert medium conveying pipe between the inert medium storage tank and the resin mixed liquid temporary storage tank;
the disperse phase feeding flowmeter is arranged on a conveying pipe II between the resin mixed liquor temporary storage tank and the first-stage reaction kettle, the thermal inert medium feeding flowmeter is arranged on a thermal inert medium conveying pipe between the inert medium heating tank and the first-stage reaction kettle, and the first-stage reaction kettle temperature sensor and the first-stage reaction kettle pressure sensor are both arranged on the pressure of the first-stage reaction kettle;
The first-stage reaction liquid feeding flowmeter is arranged on a conveying pipe III between the first-stage reaction kettle and the second-stage reaction kettle, and the second-stage reaction kettle temperature sensor and the second-stage reaction kettle pressure sensor are both arranged on the second-stage reaction kettle;
the secondary reaction liquid feeding flowmeter is arranged on a conveying pipe IV between the secondary reaction kettle and the tertiary reaction kettle, and the tertiary reaction kettle temperature sensor and the tertiary reaction kettle pressure sensor are both arranged on the tertiary reaction kettle;
the three-stage reaction liquid feeding flowmeter is arranged on a conveying pipe V between the three-stage reaction kettle and the coil pipe reactor, and the coil pipe reactor temperature sensor and the coil pipe reactor pressure sensor are both arranged on the coil pipe reactor;
the product liquid feeding flowmeter is arranged on a conveying pipe VI between the coil pipe reactor and the separating cylinder;
the cold inert medium feeding flowmeter II is arranged on a pipeline between the inert medium storage tank and the inert medium heating tank, and the inert medium heating tank temperature sensor is arranged on the inert medium heating tank;
the equipment group also comprises an epoxy resin regulating valve arranged on an epoxy resin feeding pipe, a curing agent regulating valve arranged on a curing agent feeding pipe, an accelerator regulating valve arranged on an accelerator feeding pipe, a toughening agent regulating valve arranged on a toughening agent feeding pipe, a surface auxiliary agent regulating valve arranged on a surface auxiliary agent feeding pipe, a resin mixed liquid regulating valve arranged on a conveying pipe I, a cold inert medium regulating valve arranged on a cold inert medium conveying pipe, a disperse phase regulating valve arranged on a conveying pipe II, a hot inert medium regulating valve arranged on a hot inert medium conveying pipe, a first-stage reaction liquid regulating valve arranged on a conveying pipe III, a second-stage reaction liquid regulating valve arranged on a conveying pipe IV, a third-stage reaction liquid regulating valve arranged on a conveying pipe V and a product liquid regulating valve arranged on a conveying pipe VI;
The equipment group also comprises a batching motor arranged on the batching tank, a primary reaction motor arranged on the primary reaction kettle, a secondary reaction motor arranged on the secondary reaction kettle and a tertiary reaction motor arranged on the tertiary reaction kettle.
The alarm control module is connected with an alarm lamp and a loudspeaker, and the alarm lamp and the loudspeaker are distributed in the epoxy resin fracturing propping agent preparation system; the cleaning control module is connected with cleaning pumps which are distributed in the epoxy resin fracturing propping agent preparation system.
In the technical scheme, corresponding conveying pumps, feeding valves, discharging valves, stop valves, ball valves, pressure reducing valves, drain valves, safety valves, heat preservation sleeves and the like can be arranged on corresponding pipelines according to actual demands.
In the technical proposal, the positions of the back side, the middle, the upper, the inner, the top, the middle, the lower, the bottom, the clockwise upward, the upper and the like are related, is defined according to the actual use condition, is a conventional term in the technical field, and is also a conventional term in the actual use process of a person skilled in the art.
In the description of the present technical solution, it should be noted that, unless explicitly specified and limited otherwise, terms "disposed", "connected" and "connected" should be interpreted broadly, and for example, they may be fixed, removable or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
By adopting the technical scheme, the beneficial technical effects brought are as follows:
1. according to the invention, through a corresponding preparation process and control system, the epoxy resin fracturing propping agent with excellent performance can be obtained, and the indexes of the epoxy resin fracturing propping agent are ensured to meet the following conditions: the density is less than or equal to 1.18g/cm 3 The roundness is more than or equal to 0.9, the sphericity is more than or equal to 0.9, the breakage resistance is less than or equal to 3%, the acid solubility is less than or equal to 0.2%, the size distribution range is 300-2000 mu m, and the low-density fracturing propping agent is obtained, has high breakage resistance, smooth surface and low surface energy, is beneficial to the export of oil gas, has small return discharge capacity, and can greatly improve the oil gas production efficiency. The application of the low-density epoxy resin fracturing propping agent can avoid or reduce the use of polymer fracturing fluid, reduce the post-treatment procedures of the post-fracturing fluid, effectively reduce the pollution and waste of groundwater resources, protect the health of the environment and the ecological system, and has great and profound significance;
2. the invention has high degree of automation control, and the related procedure operation can be independently completed by a control system, so that the manual labor intensity is effectively reduced, and meanwhile, the safety, low cost, stability, order, controllability and traceability of the preparation production line can be ensured, and the industrial mass production requirement is met.
Drawings
FIG. 1 is a schematic diagram of an epoxy fracturing propping agent molding principle in the present invention;
FIG. 2 is a process flow diagram of the present invention;
FIG. 3 is a schematic diagram of the apparatus arrangement of the present invention;
FIG. 4 is a schematic diagram of the structure of the material mixing tank according to the present invention;
FIG. 5 is a top view of a dosage tank of the present invention;
FIG. 6 is a schematic diagram of a temporary storage tank for resin mixed liquor in the present invention;
FIG. 7 is a top view of a resin mixed liquor temporary storage tank according to the present invention;
FIG. 8 is a schematic structural diagram of a primary reaction kettle in the invention;
FIG. 9 is a top view of the primary reaction kettle in the present invention;
FIG. 10 is a schematic structural diagram of a secondary reaction vessel according to the present invention;
FIG. 11 is a top view of a secondary reaction vessel in accordance with the present invention;
FIG. 12 is a schematic structural diagram of a three-stage reaction kettle in the invention;
FIG. 13 is a top view of a three-stage reactor according to the present invention;
FIG. 14 is a schematic view showing the structure of a coil reactor according to the present invention;
FIG. 15 is a top view of a coil reactor according to the present invention;
FIG. 16 is a schematic view of the structure of an inert medium reservoir according to the present invention;
FIG. 17 is a top view of an inert medium reservoir of the present invention;
FIG. 18 is a schematic view of the structure of an inert medium heating tank according to the present invention;
FIG. 19 is a top view of an inert media heating tank of the present invention;
FIG. 20 is a diagram of a logical connection of a control system according to the present invention;
FIG. 21 is a diagram of the logical connections between a DCS controller and a sensor cluster in the control system of the present invention;
FIG. 22 is a diagram of the logical connections of a device cluster in the control system of the present invention;
FIG. 23 is a partial circuit diagram of the present invention;
FIG. 24 is a pictorial representation of an epoxy fracturing proppant product of the present invention;
FIG. 25 is a test report (one) of an epoxy fracturing proppant product of the present invention;
FIG. 26 is a test report (II) of an epoxy fracturing proppant product of the present invention;
FIG. 27 is a graph of the successful production of an epoxy fracturing proppant involved in the production of the present invention;
FIG. 28 is a graph of failed products of epoxy fracturing proppants involved in the production of the present invention;
FIG. 29 is a state diagram of an epoxy fracturing proppant product of the present invention in an inert medium;
in the figure, 1, an epoxy resin storage tank, 2, a curing agent storage tank, 3, an accelerator storage tank, 4, a flexibilizer storage tank, 5, a surface auxiliary agent storage tank, 6, a material mixing tank, 7, a resin mixed liquid temporary storage tank, 8, a primary reaction kettle, 9, a secondary reaction kettle, 10, a tertiary reaction kettle, 11, a coil pipe reactor, 12, a separation cylinder, 13, an inert medium storage tank, 14 and an inert medium heating tank;
15. Epoxy resin feeding pipe 16, curing agent feeding pipe 17, accelerator feeding pipe 18, toughener feeding pipe 19, surface auxiliary agent feeding pipe 20, conveying pipe I, 21, cold inert medium conveying pipe 22, conveying pipe II, 23, hot inert medium conveying pipe 24, conveying pipe III, 25, conveying pipe IV, 2601, conveying pipe V, 2602, conveying pipe VI, 2603, inert medium feeding pipe 2604 and recycling pipe;
26. the system comprises a DCS controller 261, a batching control module 262, a pre-curing control module 263, a primary reaction control module 264, a secondary reaction control module 265, a tertiary reaction control module 266, a post-curing control module 267, a separation control module 268, an inert medium heating control module 269, an alarm control module 270 and a cleaning control module;
27. a human-computer interface is provided with a human-computer interface,
28. a data acquisition unit, 280, a sensor group, 2801, an epoxy resin feeding flowmeter, 2802, a curing agent feeding flowmeter, 2803, an accelerator feeding flowmeter, 2804, a toughener feeding flowmeter, 2805, a surface auxiliary feeding flowmeter, 2806, a resin mixed liquid feeding flowmeter, 2807, a cold inert medium feeding flowmeter I, 2808, a disperse phase feeding flowmeter, 2809, a hot inert medium feeding flowmeter, 2810, a primary reaction kettle temperature sensor, 2811, a primary reaction kettle pressure sensor, 2812, a primary reaction liquid feeding flowmeter, 2813, a secondary reaction kettle temperature sensor, 2814, a secondary reaction kettle pressure sensor, 2815, a secondary reaction liquid feeding flowmeter, 2816, a tertiary reaction kettle temperature sensor, 2817, a tertiary reaction kettle pressure sensor, 8, a tertiary reaction liquid feeding flowmeter, 2819, a coil reactor temperature sensor, 2820, a coil reactor pressure sensor, 2821, a product liquid feeding flowmeter, 2822, a cold inert medium feeding flowmeter II, 2823, an inert medium heating tank temperature sensor;
29. The method comprises the steps of executing units, 290, equipment groups, 2901, epoxy resin regulating valves, 2902, curing agent regulating valves, 2903, accelerator regulating valves, 2904, toughening agent regulating valves, 2905, resin mixed liquid regulating valves, 2906, cold inert medium regulating valves, 2907, disperse phase regulating valves, 2908, hot inert medium regulating valves, 2909, primary reaction liquid regulating valves, 2910, secondary reaction liquid regulating valves, 2911, tertiary reaction liquid regulating valves, 2912, product liquid regulating valves, 2913, batching motors, 2914, primary reaction motors, 2915, secondary reaction motors, 2916, tertiary reaction motors, 2917 and surface auxiliary agent regulating valves.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below by means of examples, and it is obvious that the described examples are only some, but not all, examples of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Firstly, the inventor establishes a set of low-density epoxy resin fracturing propping agent production line by researching feasibility of links such as fracturing propping agent production process, equipment, flow and the like, and solves problems and solutions possibly occurring in industrialization, the production and manufacturing flow is opened, common specification products with the particle size of 0.30-2 mm are prepared, other performance indexes meet the requirements of the fracturing propping agent, and parameters and basis are provided for the later-stage large-scale production process;
Secondly, the low-density fracturing propping agent has the effects of small return discharge amount, low sedimentation velocity and effective supporting of deep well cracks, but also has the problems of complex preparation process, higher cost and the like. The invention starts from raw materials such as epoxy resin, and prepares a series of low-density epoxy resin fracturing propping agents with different dimensions, and the low-density epoxy resin fracturing propping agents have the following advantages:
1. the density of the epoxy resin fracturing propping agent is less than or equal to 1.18g/cm 3 Roundness of 0.9, sphericity of 0.9, acid solubility of 0.2% or less, and high crushing resistance (shown in the following table 1, fig. 25 to 26); as an organic material, the surface is smooth, the surface energy is low, the export of oil gas is facilitated, and the oil gas production efficiency can be greatly improved;
2. the epoxy resin fracturing propping agent has low density, so that polymer type fracturing fluid can be used without or less, water can be directly used or the use and the transportation of the fracturing fluid are reduced, the environment-friendly treatment process and the cost of flowback fluid are reduced, and the fracturing construction process is simplified;
3. the oil-gas field in China is a low-permeability shale oil-gas field and is characterized by poor fluid permeability and low productivity, the fracturing propping agent is used as a key material of a fracturing technology, and the quality of the performance directly influences the yield of an oil-gas well (shown in figures 27 and 29);
Finally, the invention provides a formula of a compatible low-density epoxy resin fracturing propping agent product, which comprises the following components in parts by mass:
100 parts of epoxy resin, 10-100 parts of curing agent, 0.1-10 parts of accelerator, 1-30 parts of flexibilizer, 0.1-10 parts of surface auxiliary agent and 200-2000 parts of inert medium;
the indexes of the low-density epoxy resin fracturing propping agent comprise: the density is less than or equal to 1.18g/cm 3 The roundness is more than or equal to 0.9, the sphericity is more than or equal to 0.9, the breakage resistance is less than or equal to 3%, the acid solubility is less than or equal to 0.2%, and the size distribution range is 300-2000 mu m.
More specifically, the epoxy resin is one or a mixture of more than two of bisphenol A type epoxy resin E-51, bisphenol A type epoxy resin E-44, bisphenol A type epoxy resin E-20, bisphenol F type epoxy resin NPEF170, phenolic type epoxy resin F-44, phenolic type epoxy resin F-51 and multifunctional epoxy AG-80 and SK-0430. The epoxy resin is further limited, can better participate in a crosslinked network, provides excellent mechanical properties, and keeps the high breakage resistance of the epoxy resin propping agent.
More specifically, the curing agent is one or a mixture of more than two of modified hexamethylenediamine, dicyandiamide, modified imidazole, anhydride and phenolic resin. Further limitation of the curing agent can better cure raw material epoxy resin and provide a crosslinked network.
More specifically, the accelerator is one or a mixture of more than two of phenyldimethylurea, 2, 4-toluene dimethylurea, 2,4, 6-tris (dimethylaminomethyl) phenol, N-dimethylbenzylamine, triethanolamine, 2-methylimidazole and modified imidazole. The accelerator is further limited, so that the curing agent can better accelerate the curing of the raw material epoxy resin.
More specifically, the toughening agent is one or a mixture of more than two of polyether type toughening agent, polyurethane type toughening agent, polytetrahydrofuran type toughening agent, nitrile rubber toughening agent and latent polyurethane toughening agent. The toughening agent is further limited, so that a tough crosslinked network can be better provided for the cured epoxy resin, and further, the performance index of the epoxy resin fracturing propping agent is ensured, so that the actual requirement is met.
More specifically, the surface auxiliary agent is one or the mixture of more than two of polyacrylic acid, organosilicon polymer, modified polyacrylic acid and modified organosilicon. The surface auxiliary agent is further limited, so that the epoxy resin mixed solution can be well assisted to be spherical and dispersed in an inert medium.
More specifically, the inert medium is one or a mixture of more than two of soybean oil, palm oil and methyl silicone oil (viscosity 1000-10000 mPa.s). Further limitation of the inert medium can better provide the environment for molding the product and ensure that the epoxy resin dispersed into the sphere is solidified and molded into the sphere-shaped particles (shown in figure 1).
In order to obtain the low-density epoxy resin fracturing propping agent, the index density is less than or equal to 1.18g/cm 3 The roundness is more than or equal to 0.9, sphericity is more than or equal to 0.9, breakage resistance is less than or equal to 3%, acid solubility is less than or equal to 0.2%, size distribution range is 300-2000 μm, industrial, automatic and economical mass production is realized, the invention is further described in detail with reference to examples, but the embodiment of the invention is not limited to the above.
Example 1
The present embodiment provides: a process for preparing a fracturing propping agent suitable for low-density epoxy resin, as shown in fig. 2, comprises the following steps:
s1, proportioning: respectively feeding epoxy resin, a curing agent, an accelerator, a toughening agent and a surface auxiliary agent into a batching tank, and stirring and mixing under the conditions of normal temperature and normal pressure to obtain a resin mixed solution;
s2, pre-curing: introducing cold inert medium in an inert medium storage tank into a resin mixed solution temporary storage tank, then introducing the resin mixed solution in a preparation tank into the resin mixed solution temporary storage tank, and controlling the content of the resin mixed solution in each liter of cold inert medium to be 0.05-0.5 kg, so as to disperse phases;
s3, heating: introducing cold inert medium into an inert medium heating tank, and heating to obtain hot inert medium;
S4, primary reaction: controlling the introduction of a thermal inert medium into the first-stage reaction kettle, controlling the introduction of a dispersion phase into the first-stage reaction kettle after the temperature of the thermal inert medium in the first-stage reaction kettle is stabilized at 100-150 ℃, and performing first-stage reaction to obtain a first-stage reaction liquid with the size distribution range of 3-6 mm;
s5 secondary reaction: the primary reaction liquid is controlled to be introduced into a secondary reaction kettle for secondary reaction, and the secondary reaction liquid with the size distribution range of 0.30-2 mm is controlled;
s6, three-stage reaction: the second-stage reaction liquid is controlled to be introduced into a third-stage reaction kettle for third-stage reaction, and the third-stage reaction liquid is controlled to be obtained;
s7, post-curing: the third-stage reaction liquid is controlled to be introduced into a coil reactor, and is subjected to pipeline post-curing to obtain completely cured product liquid;
s8, separation: and (3) controlling to introduce the completely solidified product liquid into a separation cylinder, and filtering through a filter screen in the separation cylinder to obtain the epoxy resin fracturing propping agent (shown in figure 24).
Example 2
On the basis of example 1, this example further defines, in order to ensure the controllability, the order and the stability of the preparation process:
the charging flow rates of the epoxy resin, the curing agent, the accelerator, the toughening agent and the surface auxiliary agent are respectively 450-550 cm 3 /min、450～550cm 3 /min、200～300cm 3 /min、100～200 cm 3 Per minute and 50-100 cm 3 /min；
The feeding flow of the cold inert medium is 120-140 cm 3 /min；
The feeding flow of the resin mixed solution is 450-550 cm 3 /min；
The feeding flow of the thermal inert medium is 800-1200 cm 3 /min；
The feeding flow of the disperse phase is 100-200 cm 3 /min；
The feeding flow of the primary reaction is 180-220 cm 3 /min；
The feeding flow of the secondary reaction liquid is 230-270 cm 3 /min；
The feeding flow of the tertiary reaction liquid is 120-180 cm 3 /min；
The feeding flow of the completely solidified product liquid is 180-220 cm 3 /min。
Wherein, the first-stage reaction kettle, the second-stage reaction kettle and the third-stage reaction kettle are all 50L.
Example 3
On the basis of examples 1-2, this example further defines, in order to ensure high quality and high efficiency of the preparation process:
in the batching process of step S1, control: the epoxy resin, the curing agent, the accelerator, the toughening agent and the surface auxiliary agent are calculated according to parts by weight, and the proportioning relationship is 100: 10-100: 0.1 to 10: 1-30: 0.1 to 10, and stirring rotation speed of 30 to 100r/min and stirring time of 20 to 40min;
in the heating step of step S3, control: heating the cold inert medium at 100-150 ℃ and normal pressure; wherein, set up electric heater: 380V of power supply, 28KW of thermal power;
in the primary reaction step of step S4, control: stirring at 100-150 deg.c and rotation speed of 80-120 r/min and pressure of 0.08-0.12 MPa to perform first stage reaction;
In the secondary reaction step of step S5, control: stirring at 100-150 deg.c and rotation speed of 80-120 r/min and pressure of 0.08-0.12 MPa to perform secondary reaction;
in the three-stage reaction process of step S6, control: stirring at 100-150 deg.c and rotation speed of 80-120 r/min and pressure of 0.08-0.12 MPa to perform three-stage reaction;
in the post-curing step of step S7, control: performing post-curing on the pipeline at the temperature of 100-150 ℃ and under normal pressure;
wherein, the mesh number of the filter screen in the separating cylinder is 10-50 meshes, and the definition of the pore diameter of the filter screen is better matched with the size of the epoxy resin fracturing propping agent product. And, according to the actual demand, the hierarchical filtration.
Example 4
On the basis of the embodiments 1-3, in order to realize recycling of the inert medium, the embodiment is further defined as follows:
the filtered inert medium is directly recycled to the inert medium heating tank to complete the continuous production process, on one hand, the recycling of the inert medium is realized, and on the other hand, the recycling of heat energy is realized, namely, the energy consumption of the electric heater is reduced, and the recycling economy and the environmental protection economy are realized.
Example 5
The embodiment provides a preparation system suitable for a low-density epoxy resin fracturing propping agent, as shown in fig. 2-3, so as to match with a preparation process of the low-density epoxy resin fracturing propping agent, which specifically comprises the following steps:
The system comprises an epoxy resin storage tank 1, a curing agent storage tank 2, an accelerator storage tank 3, a flexibilizer storage tank 4, a surface auxiliary agent storage tank 5, a batching tank 6, a resin mixed liquid temporary storage tank 7, a first-stage reaction kettle 8, a second-stage reaction kettle 9, a third-stage reaction kettle 10, a coil reactor 11 and a separating cylinder 12, wherein the epoxy resin storage tank 1 is connected with the batching tank 6 through an epoxy resin feeding pipe 15, the curing agent storage tank 2 is connected with the batching tank 6 through a curing agent feeding pipe 16, the accelerator storage tank 3 is connected with the batching tank 6 through an accelerator feeding pipe 17, the flexibilizer storage tank 4 is connected with the batching tank 6 through a flexibilizer feeding pipe 18, and the surface auxiliary agent storage tank 5 is connected with the batching tank 6 through a surface auxiliary agent feeding pipe 19;
the discharge port of the batching tank 6 is connected with the feed port of the resin mixed liquid temporary storage tank 7 through a conveying pipe I20, and the resin mixed liquid temporary storage tank 7 is arranged at the rear side of a station of the batching tank 6; the feed inlet of the resin mixed liquor temporary storage tank 7 is also connected with a cold inert medium conveying pipe 21; the discharge port of the resin mixed solution temporary storage tank 7 is connected with the feed port of the first-stage reaction kettle 8 through a conveying pipe II 22, the first-stage reaction kettle 8 is arranged at the rear side of the station of the resin mixed solution temporary storage tank 7, and the first-stage reaction kettle 8 is connected with a thermal inert medium conveying pipe 23; the discharge port of the primary reaction kettle 8 is connected with the feed port of the secondary reaction kettle 9 through a conveying pipe III 24, and the secondary reaction kettle 9 is arranged at the rear side of the station of the primary reaction kettle 8; the discharge port of the secondary reaction kettle 9 is connected with the feed port of the tertiary reaction kettle 10 through a conveying pipe IV 25, and the tertiary reaction kettle 10 is arranged at the rear side of a station of the secondary reaction kettle 9; the discharge port of the three-stage reaction kettle 10 is connected with the feed port of a coil reactor 11 through a conveying pipe V2601, and the coil reactor 11 is arranged at the rear side of a station of the three-stage reaction kettle 10; the discharge port of the coil reactor 11 is connected with the feed port of a separating cylinder 12 through a conveying pipe VI 2602, and the separating cylinder 12 is arranged at the rear side of a station of the coil reactor 11; a discharge hole of the separating cylinder 12 is connected with an epoxy resin fracturing propping agent temporary storage tank;
A continuous passage for preparing the epoxy resin fracturing propping agent is formed among the material mixing tank 6, the resin mixed liquid temporary storage tank 7, the primary reaction kettle 8, the secondary reaction kettle 9, the tertiary reaction kettle 10, the coil pipe reactor 11 and the separating cylinder 12;
wherein, batching jar 6: as shown in fig. 4-5, a frame stirrer is arranged in the device, the frame stirrer is connected with a vertical gear reducer and a frequency converter, an epoxy resin feed port, a curing agent feed port, an accelerator feed port and a standby port/exhaust port are arranged at the top, a sight glass port is arranged at the middle part, and a discharge port is arranged at the lower part;
resin mixed solution temporary storage tank 7: as shown in fig. 6-7, the feed inlet of the temporary storage tank 7 for the resin mixed liquor is arranged at the top of the temporary storage tank 7 for the resin mixed liquor, the top is also provided with a standby port, an emptying port and a cold inert medium inlet, and the bottom is provided with a dispersed phase outlet;
primary reaction kettle 8: as shown in fig. 8-9, a frame stirrer is arranged in the frame stirrer, and the transverse blade in the frame stirrer turns upwards clockwise at 45 degrees; the surface of the stirrer needs to be coated with a release agent; the frame type stirrer is connected with a vertical gear reducer and a frequency converter; the discharge port of the first-stage reaction kettle 8 is arranged at the upper part of the first-stage reaction kettle 8, the middle part is provided with a sight glass port and a first-stage reaction liquid outlet, and the lower part is provided with a disperse phase inlet, a thermal inert medium inlet and an emptying port;
Secondary reaction kettle 9: as shown in fig. 10-11, a frame stirrer is arranged in the frame stirrer, and the transverse blade in the frame stirrer turns upwards clockwise at 45 degrees; the surface of the stirrer needs to be coated with a release agent; the frame type stirrer is connected with a vertical gear reducer and a frequency converter; the discharge port of the secondary reaction kettle 9 is arranged at the upper part of the secondary reaction kettle 9, the top of the secondary reaction kettle is provided with a vent, and an internal thread ball valve is sleeved in the vent; the middle part is provided with a sight glass opening and a secondary reaction liquid outlet, and the lower part is provided with a primary reaction liquid inlet;
three-stage reaction kettle 10: as shown in fig. 12-13, a double helical ribbon stirrer is arranged in the double helical ribbon stirrer, and the double helical ribbon turns upwards clockwise; the surface of the stirrer needs to be coated with a release agent; the double helical ribbon stirrer is connected with a vertical gear reducer and a frequency converter; the discharge port of the three-stage reaction kettle 10 is arranged at the upper part of the three-stage reaction kettle 10, the upper part is provided with a three-stage reaction liquid outlet, the top is provided with a vent, and an internal thread ball valve is sleeved in the vent; the lower part is provided with a secondary reaction liquid inlet;
coil reactor 11: as shown in fig. 14-15, the top is connected by adopting an integral movable cover and a bolt; the heat insulating material is perlite or rock wool, the upper part is provided with a three-stage reaction liquid inlet, and the lower part is provided with a product liquid outlet.
Further, the temporary storage tank 7 for the resin mixed liquor is connected with an inert medium storage tank 13 through a cold inert medium conveying pipe 21, the inert medium storage tank 13 is connected with an inert medium heating tank 14 through an inert medium inlet pipe 2603, and the inert medium heating tank 14 is connected with the primary reaction kettle 8 through a hot inert medium conveying pipe 23;
Wherein the inert medium storage tank 13: as shown in fig. 16-17, the top is connected by a half-open movable cover and a bolt; the upper part is provided with an overflow port, and the lower part is provided with a cold inert medium outlet;
inert medium heating tank 14: as shown in fig. 18-19, the thermal insulation material is perlite or rock wool, the upper part is provided with a cold inert medium inlet, a return port, a vent, an overflow port and a circulation port, and the lower part is provided with a hot inert medium outlet.
Further, an inert medium outlet on the separation cylinder 12 is connected with a reflux inlet of the inert medium heating pot 14 through a recovery pipe 2604.
Further, at least two separating drums 12, a discharge hole of the coil reactor 11 is connected with a feed hole of the first-stage separating drum 12, a discharge hole of the first-stage separating drum 12 is connected with a next-stage separating feed hole, the separating drums 12 are sequentially connected, and a discharge hole of the last-stage separating drum is connected with an epoxy resin fracturing propping agent temporary storage tank. And the hierarchical filtration can be performed according to actual requirements.
Example 6
The embodiment provides a control system suitable for the low-density epoxy resin fracturing propping agent on the basis of a preparation system of the low-density epoxy resin fracturing propping agent, so as to match with the preparation process of the low-density epoxy resin fracturing propping agent.
As shown in fig. 20 and 23, the control system includes a DCS controller 26, where the DCS controller 26 is connected to a human-computer interface 27 through a data input interface, the DCS controller 26 is connected to a data acquisition unit 28 through a data feedback interface, and the DCS controller 26 is connected to an execution unit 29 through a data output interface;
1) DCS controller 26: comprises a batching control module 261, a pre-curing control module 262, a primary reaction control module 263, a secondary reaction control module 264, a tertiary reaction control module 265, a post-curing control module 266 and a separation control module 267;
2) Data acquisition unit 28: the data acquisition unit 28 includes a sensor cluster 280 for data acquisition and transmission in the epoxy fracturing proppant manufacturing process, as provided in the epoxy fracturing proppant manufacturing system. According to the actual requirements, it is preferable that the sensor group 280 includes an epoxy resin feeding flow meter 2801, a curing agent feeding flow meter 2802, an accelerator feeding flow meter 2803, a toughening agent feeding flow meter 2804 and a surface auxiliary agent feeding flow meter 2805 connected with the batching control module 261, a resin mixed liquid feeding flow meter 2806 and a cold inert medium feeding flow meter i 2807 connected with the pre-curing control module 262, a dispersed phase feeding flow meter 2808, a hot inert medium feeding flow meter 2809, a primary reaction kettle temperature sensor 2810 and a primary reaction kettle pressure sensor 2811 connected with the secondary reaction control module 264, a primary reaction liquid feeding flow meter 2812, a secondary reaction kettle temperature sensor 2813 and a secondary reaction kettle pressure sensor 2814 connected with the tertiary reaction control module 265, a secondary reaction liquid feeding flow meter 2815, a tertiary reaction kettle temperature sensor 2816 and a tertiary reaction kettle pressure sensor 2817 connected with the post-curing control module 262, a tertiary reaction liquid feeding flow meter 2818, a coil pipe temperature sensor 2819 and a secondary reaction kettle pressure sensor 28120 connected with the post-curing control module 266, and a cold inert medium feeding flow meter 2823 connected with the secondary reaction control module 2820.
3) Execution unit 29: disposed in the epoxy fracturing proppant preparation system, the execution unit 29 includes a cluster 290 of equipment for epoxy fracturing proppant preparation and conditioning. According to the actual requirements, it is preferable that the equipment group 290 is further defined, that is, as shown in fig. 2, 3 and 22, the equipment group 290 includes an epoxy resin storage tank 1, a curing agent storage tank 2, an accelerator storage tank 3, a toughener storage tank 4, a surface auxiliary agent storage tank 5, a batching tank 6, a resin mixed liquor temporary storage tank 7, a primary reaction kettle 8, a secondary reaction kettle 9, a tertiary reaction kettle 10, a coil reactor 11 and a separating cylinder 12, an epoxy resin feeding flow meter 2801 is arranged on an epoxy resin feeding pipe 15 between the epoxy resin storage tank 1 and the batching tank 6, a curing agent feeding flow meter 2802 is arranged on a curing agent feeding pipe 16 between the curing agent storage tank 2 and the batching tank 6, an accelerator feeding flow meter 2803 is arranged on an accelerator feeding pipe 17 between the accelerator storage tank 3 and the batching tank 6, a toughener feeding flow meter 2804 is arranged on a toughener feeding pipe 18 between the toughener storage tank 4 and the batching tank 6, and a surface auxiliary agent feeding meter 2805 is arranged on a surface auxiliary agent feeding pipe 19 between the surface auxiliary agent storage tank 5 and the batching tank 6; the resin mixed liquor feeding flowmeter 2806 is arranged on a conveying pipe I20 between the batching tank 6 and the resin mixed liquor temporary storage tank 7, and the cold inert medium feeding flowmeter I2807 is arranged on a cold inert medium conveying pipe 21 between the inert medium storage tank 13 and the resin mixed liquor temporary storage tank 7; a disperse phase feeding flowmeter 2808 is arranged on a conveying pipe II 22 between the resin mixed liquor temporary storage tank 7 and the first-stage reaction kettle 8, a thermal inert medium feeding flowmeter 2809 is arranged on a thermal inert medium conveying pipe 23 between the inert medium heating tank 14 and the first-stage reaction kettle 8, and a first-stage reaction kettle temperature sensor 2810 and a first-stage reaction kettle pressure sensor 2811 are both arranged on the pressure of the first-stage reaction kettle 8; a primary reaction liquid feeding flowmeter 2812 is arranged on a conveying pipe III 24 between the primary reaction kettle 8 and the secondary reaction kettle 9, and a secondary reaction kettle temperature sensor 2813 and a secondary reaction kettle pressure sensor 2814 are both arranged on the secondary reaction kettle 9; a secondary reaction liquid feeding flowmeter 2815 is arranged on a conveying pipe IV 25 between the secondary reaction kettle 9 and the tertiary reaction kettle 10, and a tertiary reaction kettle temperature sensor 2816 and a tertiary reaction kettle pressure sensor 2817 are both arranged on the tertiary reaction kettle 10; a three-stage reaction liquid feeding flowmeter 2818 is arranged on a conveying pipe V2601 between the three-stage reaction kettle 10 and a coil reactor 11, and a coil reactor temperature sensor 2819 and a coil reactor pressure sensor 2820 are both arranged on the coil reactor 11; a product liquid feeding flowmeter 2821 is arranged on a conveying pipe VI 2602 between the coil pipe reactor 11 and the separating cylinder 12; a cold inert medium feeding flowmeter II 2822 is arranged on a pipeline between the inert medium storage tank 13 and the inert medium heating tank 14, and an inert medium heating tank temperature sensor 2823 is arranged on the inert medium heating tank 14;
And, the equipment group 290 further includes an epoxy resin regulating valve 2901 provided on the epoxy resin feed pipe 15, a curing agent regulating valve 2902 provided on the curing agent feed pipe 16, an accelerator regulating valve 2903 provided on the accelerator feed pipe 17, a toughening agent regulating valve 2904 provided on the toughening agent feed pipe 18, a surface auxiliary agent regulating valve 2917 provided on the surface auxiliary agent feed pipe 19, a resin mixed liquid regulating valve 2905 provided on the conveying pipe i 20, a cold inert medium regulating valve 2906 provided on the cold inert medium conveying pipe 21, a dispersed phase regulating valve 2907 provided on the conveying pipe ii 22, a hot inert medium regulating valve 2908 provided on the hot inert medium conveying pipe 23, a primary reaction liquid regulating valve 2909 provided on the conveying pipe iii 24, a secondary reaction liquid regulating valve 2910 provided on the conveying pipe iv 25, a tertiary reaction liquid regulating valve 2601 provided on the conveying pipe v 2602911, a product liquid regulating valve 2602 provided on the conveying pipe vi 2;
and, the equipment group 290 further comprises a batching motor 2913 arranged on the batching tank 6, a first-stage reaction motor 2914 arranged on the first-stage reaction kettle 8, a second-stage reaction motor 2915 arranged on the second-stage reaction kettle 9 and a third-stage reaction motor 2916 arranged on the third-stage reaction kettle 10.
In order to further improve the automation and the stability of the preparation process of the low-density epoxy resin fracturing propping agent, the preparation method is also provided with the following steps: the DCS controller 26 further comprises an alarm control module 269, a purge control module 270 and an inert medium heating control module 268, wherein the alarm control module 269 is connected with alarm lamps and microphones distributed in the epoxy resin fracturing proppant production system; the purge control module 270 is connected with purge pumps distributed in the epoxy fracturing proppant preparation system.
Example 7
Based on embodiment 6, the embodiment provides a control method of a matched low-density epoxy resin fracturing propping agent, which specifically comprises the following steps:
A. respectively feeding epoxy resin, a curing agent, an accelerator, a toughening agent and a surface auxiliary agent into a batching tank 6, and controlling an epoxy resin feeding flowmeter 2801 by a batching control module 261 to detect the addition amount of the epoxy resin and send a signal of the addition amount of the epoxy resin to a DCS controller 26; the batching control module 261 controls the curing agent feeding flowmeter 2802 to detect the addition amount of the curing agent and send a signal of the curing agent addition amount to the DCS controller 26; the compounding control module 261 controls the accelerator feed flow meter 2803 to detect the amount of accelerator added and signals the amount of accelerator added to the DCS controller 26; the batching control module 261 controls the toughening agent feeding flowmeter 2804 to detect the addition amount of the toughening agent and send a signal of the addition amount of the toughening agent to the DCS controller 26; the ingredient control module 261 controls the surface auxiliary agent feeding flowmeter 2805 to detect the addition amount of the surface auxiliary agent and send a signal of the addition amount of the surface auxiliary agent to the DCS controller 26;
When the epoxy resin, the curing agent, the accelerator, the toughening agent and the surface auxiliary agent are calculated according to parts by weight, the proportioning relationship is 100: 10-100: 0.1 to 10: 1-30: 0.1-10, the batching control module 261 controls mixing (e.g. controlling stirring speed and stirring time through the batching motor 2913);
when the parts by weight of the epoxy resin, the curing agent, the accelerator, the toughening agent and the surface auxiliary agent are not in the above proportioning relationship, the batching control module 261 sends a command of adjusting small or large to the epoxy resin adjusting valve 2901, the curing agent adjusting valve 2902, the accelerator adjusting valve 2903, the toughening agent adjusting valve 2904 and/or the surface auxiliary agent adjusting valve 2917 until the parts by weight of the epoxy resin, the curing agent, the accelerator, the toughening agent and the surface auxiliary agent are in the above proportioning relationship;
B. introducing the mixed resin mixed solution into a resin mixed solution temporary storage tank 7, controlling a resin mixed solution feeding flowmeter 2806 by a pre-curing control module 262 to detect the adding amount of the resin mixed solution, and sending a signal of the adding amount of the resin mixed solution to a DCS controller 26; the pre-cure control module 262 controls the cold inert medium feed flow meter I2807 to detect the addition of cold inert medium and signal the addition of cold inert medium to the DCS controller 26;
When the content of the resin mixed liquor in each liter of cold inert medium is higher than or lower than 0.05-0.5 kg, the pre-curing control module 262 sends a command of reducing or increasing to the resin mixed liquor regulating valve 2905 or/and the cold inert medium regulating valve 2906 until each liter of cold inert medium contains 0.05-0.5 kg of resin mixed liquor;
C. introducing the dispersion phase obtained after the pre-solidification into a first-stage reaction kettle 8, wherein a first-stage reaction control module 263 controls a dispersion phase feeding flowmeter 2808 to detect the addition amount of the dispersion phase, and sends a signal of the addition amount of the dispersion phase to a DCS controller 26; the primary reaction control module 263 controls the thermal inert medium feed flow meter 2809 to detect the amount of thermal inert medium added and signal the amount of thermal inert medium added to the DCS controller 26; the primary reaction control module 263 controls the primary reaction kettle temperature sensor 2810 to detect the temperature in the primary reaction kettle 8 and sends a signal of the temperature in the primary reaction kettle 8 to the DCS controller 26; the primary reaction control module 263 controls the primary reaction kettle pressure sensor 2811 to detect the pressure in the primary reaction kettle 8 and sends a signal of the pressure in the primary reaction kettle 8 to the DCS controller 26;
when the size of the primary reaction liquid is more than or less than 3-6 mm, the primary reaction control module 263 sends a command of reducing or enlarging to the disperse phase regulating valve 2907, the thermal inert medium regulating valve 2908 or/and the primary reaction motor 2914 until the size range of the primary reaction liquid is distributed at 3-6 mm;
D. Introducing the primary reaction liquid obtained after the primary reaction into a secondary reaction kettle 9, and controlling a primary reaction liquid feeding flowmeter 2812 by a secondary reaction control module 264 to detect the adding amount of the primary reaction liquid and send a signal of the adding amount of the primary reaction liquid to a DCS controller 26; the secondary reaction control module 264 controls the secondary reaction kettle temperature sensor 2813 to detect the temperature in the secondary reaction kettle 9 and sends a signal of the temperature in the secondary reaction kettle 9 to the DCS controller 26; the secondary reaction control module 264 controls the secondary reaction kettle pressure sensor 2814 to detect the pressure in the secondary reaction kettle 9 and send a signal of the pressure in the secondary reaction kettle 9 to the DCS controller 26;
when the size of the secondary reaction liquid is larger than or smaller than 0.30-2 mm, the secondary reaction control module 264 sends a command of reducing or enlarging to the primary reaction liquid regulating valve 2909 and/or the secondary reaction motor 2915 until the size range of the secondary reaction liquid is distributed at 0.30-2 mm;
E. the secondary reaction liquid obtained after the secondary reaction is introduced into a tertiary reaction kettle 10, and a tertiary reaction control module 265 controls a secondary reaction liquid feeding flowmeter 2815 to detect the adding amount of the secondary reaction liquid and sends a signal of the adding amount of the secondary reaction liquid to a DCS controller 26; the tertiary reaction control module 265 controls a tertiary reaction kettle temperature sensor 2816 to detect the temperature in the secondary reaction kettle 9 and send a signal of the temperature in the tertiary reaction kettle 10 to the DCS controller 26; the three-stage reaction control module 265 controls a three-stage reaction kettle pressure sensor 2817 to detect the pressure in the three-stage reaction kettle 10 and send a signal of the pressure in the three-stage reaction kettle 10 to the DCS controller 26;
Meanwhile, the tertiary reaction control module 265 can send a command of decreasing or increasing to the secondary reaction liquid adjusting valve 2910 and/or the tertiary reaction motor 2916 until a reference value is set to meet the actual requirement, for example: controlling the stirring rotation speed to be 80-120 r/min, the pressure to be 0.08-0.12 Mpa, and the like;
F. introducing the three-stage reaction liquid obtained after the three-stage reaction into a coil reactor 11, controlling a three-stage reaction liquid feeding flowmeter 2818 by a post-curing control module 266 to detect the adding amount of the three-stage reaction liquid, and sending a signal of the adding amount of the three-stage reaction liquid to a DCS controller 26; the post cure control module 266 controls the coil reactor temperature sensor 2819 to detect the temperature inside the coil reactor 11 and signals the temperature inside the coil reactor 11 to the DCS controller 26; the post-cure control module 266 controls the coil reactor pressure sensor 2820 to detect the pressure within the coil reactor 11 and signal the pressure within the coil reactor 11 to the DCS controller 26;
meanwhile, the post-curing control module 266 can send a command for adjusting the volume of the reaction liquid 2911 to the three-stage reaction liquid adjusting valve 2911 until the reference value is set to meet the actual requirement, for example: controlling the temperature to be 100-150 ℃ and the normal pressure;
G. Introducing the product liquid obtained after post-solidification into the separating cylinder 12, controlling a product liquid feeding flowmeter 2821 by a separating control module 267 to detect the adding amount of the product liquid, and sending a signal of the adding amount of the product liquid to a DCS controller 26;
meanwhile, the separation control module 267 can send a command for adjusting the volume of the product liquid 2912 to a reference value set for meeting the actual requirement, for example: ensuring the smoothness and the temperature performance of the separation process.
In addition, the control of inert medium heating in the inert medium heating tank 14, the primary reaction kettle 8, the secondary reaction kettle 9, the tertiary reaction kettle 10 and the coil pipe reactor 11 can be realized by adopting the prior mature technology, such as: and a heating jacket is sleeved outside the corresponding equipment, heating medium (the heating medium comes from a heating system) is introduced into the heating jacket, and the temperature is adjusted according to the corresponding temperature sensor and control valve so as to meet the actual requirements.
Example 8
Based on embodiments 6-7, the embodiment provides a control method of a matched low-density epoxy resin fracturing propping agent, which specifically comprises the step of controlling the cleaning of a preparation system.
After the product liquid is separated and collected, closing a heating system and a discharge valve on the batching tank 6;
adding inert media (such as soybean oil, palm oil and methyl silicone oil) into a batching tank 6, stirring and flushing the batching tank 6, opening a discharge valve on the batching tank 6 and a feed valve on a resin mixed solution temporary storage tank 7, flushing residual resin in the batching tank 6, and then introducing flushing fluid in the batching tank 6 into the resin mixed solution temporary storage tank 7;
opening a discharge valve and an inert medium feed valve on the resin mixed solution temporary storage tank 7 and a feed valve on the first-stage reaction kettle 8, flushing the resin mixed solution temporary storage tank 7, and then introducing flushing fluid in the resin mixed solution temporary storage tank 7 into the first-stage reaction kettle 8;
opening a discharge valve on the primary reaction kettle 8, a feed valve on the secondary reaction kettle 9 and an inert medium feed valve, cleaning the primary reaction kettle 8 by adopting flushing liquid in the resin mixed solution temporary storage tank 7, and then introducing the flushing liquid in the primary reaction kettle 8 into the secondary reaction kettle 9;
opening a discharge valve on the secondary reaction kettle 9 and a feed valve on the tertiary reaction kettle 10, cleaning the secondary reaction kettle 9 by adopting flushing fluid in the primary reaction kettle 8, and then introducing the flushing fluid in the secondary reaction kettle 9 into the tertiary reaction kettle 10;
Opening a discharge valve on the three-stage reaction kettle 10 and a feed valve on the coil pipe reactor 11, cleaning the three-stage reaction kettle 10 by adopting flushing fluid in the second-stage reaction kettle 9, and then introducing the flushing fluid in the three-stage reaction kettle 10 into the coil pipe reactor 11;
opening a discharge valve on the coil reactor 11 and a feed valve on the separating cylinder 12, cleaning the coil reactor 11 by adopting flushing fluid in the three-stage reaction kettle 10, and then introducing the flushing fluid in the coil reactor 11 into the separating cylinder 12;
opening a discharge valve on the separating cylinder 12 and a reflux valve on the inert medium heating tank 14, cleaning the separating cylinder 12 by adopting flushing liquid in the coil pipe reactor 11, and then refluxing the flushing liquid in the separating cylinder 12 into the inert medium heating tank 14, namely directly recycling the inert medium into the inert medium heating tank 14; meanwhile, a liquid level meter on the inert medium heating tank 14 is observed, if the liquid level is 4/5, a reflux valve on the inert medium storage tank 13 is opened, inert medium in the inert medium heating tank 14 is conveyed to the inert medium storage tank 13, and surplus inert medium is circulated back into the inert medium storage tank 13, so that the stability, smoothness and order of the whole cleaning control process are ensured;
and finally, opening the corresponding emptying valve, and placing a collecting barrel below the corresponding valve to collect residual materials in the pipeline.
Discussion examples 1-6
On the basis of example 1, the present discussion is about the influencing factors such as the raw material types, inert medium types (providing a ball forming environment for the fracturing propping agent), proportioning relation, control conditions and the like involved in the preparation process of the low-density epoxy resin fracturing propping agent, so as to further explain the present invention, and the obtained results are shown in the following table 2:
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when the epoxy resin mixed solution passes through a cold inert medium, the epoxy resin mixed solution enters a first-stage reaction kettle in a dispersed phase after being pre-solidified; mixing and stirring the epoxy resin mixed solution and a thermal inert medium in a first-stage reaction kettle, dispersing the epoxy resin mixed solution into spherical epoxy resin mixed solution, and then, driving the spherical epoxy resin mixed solution to enter a next-stage reaction kettle through the inert medium, and continuing dispersing and curing forming;
from table 2 above, it can be seen that: in the preparation of proppants by the above process, the stirring speed has a significant effect on the proppant particle size. When the stirring speed is 120r/min, the size distribution of the proppant particles is wider, the size is smaller, and the minimum size can reach 0.15mm, because the stirring blade has shearing force on the resin glue solution in the rapid stirring process; when the stirring speed is too high, the resin glue solution is subjected to larger shearing force and more shearing times, so that the particle size of the propping agent product particles is small. However, when the stirring speed is too slow, for example, 80r/min and 90r/min, the proppant product particles have a larger particle size and a narrower size distribution because the resin dope is subjected to a smaller shearing force and a limited number of shearing times. For this purpose, a proper stirring speed is selected to achieve the proppant particle size meeting the requirements; as also shown in Table 2 above, as discussed in example 3, when the primary stirring speed was 80r/min, the secondary stirring speed was 95r/min, and the tertiary stirring speed was 105r/min, it was possible to obtain a fracturing propping agent particle size (0.4-1.2 mm) meeting the requirements, and as shown in the test report, the propping agent particle size (0.4-0.8 mm) was about 98% of the product.
And, in the course of the discussion of influencing factors, the failed product involved is shown in FIG. 28.
In addition, the influencing factors are not limited to the epoxy resin formulation, reaction temperature, resin mixture feed amount, inert medium feed amount, stirring speed, etc., and will not be discussed one by one.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent variation, etc. of the above embodiment according to the technical matter of the present invention fall within the scope of the present invention.
Claims (14)
1. The preparation process of the low-density epoxy resin fracturing propping agent is characterized by comprising the following steps of:
s1, proportioning: respectively feeding epoxy resin, a curing agent, an accelerator, a toughening agent and a surface auxiliary agent into a material mixing tank, and mixing to obtain a resin mixed solution;
wherein, the control is calculated by the weight parts of epoxy resin, curing agent, accelerator, toughening agent and surface auxiliary agent, the proportioning relationship is 100: 10-100: 0.1 to 10: 1-30: 0.1 to 10, the mixing stirring speed is 30 to 100r/min, and the stirring time is 20 to 40min;
s2, pre-curing: introducing cold inert medium in an inert medium storage tank into a resin mixed solution temporary storage tank, introducing resin mixed solution in a preparation tank into the resin mixed solution temporary storage tank, and controlling the content of 0.05-0.5 kg of resin mixed solution in each liter of cold inert medium to disperse phases;
S3, heating: introducing cold inert medium into an inert medium heating tank, and heating to obtain hot inert medium;
wherein, the cold inert medium is controlled to be heated at 100-150 ℃ and normal pressure;
s4, primary reaction: introducing a thermal inert medium into a first-stage reaction kettle, controlling the dispersion phase to be introduced into the first-stage reaction kettle after the temperature of the thermal inert medium in the first-stage reaction kettle is stabilized at 100-150 ℃, and performing first-stage reaction to obtain a first-stage reaction liquid with the size distribution range of 3-6 mm;
wherein, stirring is carried out under the conditions of 100-150 ℃, the rotating speed of 80-120 r/min and the pressure of 0.08-0.12 MPa, and the primary reaction is carried out;
s5 secondary reaction: introducing the first-stage reaction liquid into a second-stage reaction kettle for a second-stage reaction, and controlling the size distribution range to be 0.30-2 mm;
wherein, stirring is carried out under the conditions of 100-150 ℃, the rotating speed of 80-120 r/min and the pressure of 0.08-0.12 MPa, and the secondary reaction is carried out;
s6, three-stage reaction: introducing the second-stage reaction liquid into a third-stage reaction kettle for third-stage reaction;
wherein, stirring is carried out under the conditions of 100-150 ℃, the rotating speed of 80-120 r/min and the pressure of 0.08-0.12 MPa, and three-stage reaction is carried out;
S7, post-curing: introducing the tertiary reaction liquid into a coil reactor, and performing pipeline post-curing to obtain a completely cured product liquid;
wherein, the post-curing of the pipeline is carried out under the conditions of 100-150 ℃ and normal pressure;
s8, separation: and (3) introducing the completely solidified product liquid into a separating cylinder, and filtering through a filter screen in the separating cylinder to obtain the epoxy resin fracturing propping agent.
2. The process for preparing a low density epoxy resin fracturing propping agent according to claim 1, wherein the indexes of the epoxy resin fracturing propping agent comprise: the density is less than or equal to 1.18g/cm 3 The roundness is more than or equal to 0.9, the sphericity is more than or equal to 0.9, the breakage resistance is less than or equal to 3%, the acid solubility is less than or equal to 0.2%, and the size distribution range is 300-2000 mu m.
3. The process for preparing the low-density epoxy resin fracturing propping agent according to claim 1, wherein,
the charging flow rates of the epoxy resin, the curing agent, the accelerator, the toughening agent and the surface auxiliary agent are respectively 450-550 cm 3 /min、450～550cm 3 /min、200～300cm 3 /min、100～200 cm 3 Per minute and 50-100 cm 3 /min；
The feeding flow of the cold inert medium is 120-140 cm 3 /min；
The feeding flow of the resin mixed solution is 450-550 cm 3 /min；
The feeding flow of the thermal inert medium is 800-1200 cm 3 /min；
The feeding flow of the disperse phase is 100-200 cm 3 /min；
The feeding flow of the primary reaction is 180-220 cm 3 /min；
The feeding flow of the secondary reaction liquid is 230-270 cm 3 /min；
The feeding flow of the tertiary reaction liquid is 120-180 cm 3 /min；
The feeding flow of the completely solidified product liquid is 180-220 cm 3 /min。
4. The process for preparing a low-density epoxy resin fracturing propping agent according to claim 1, wherein in step S8, the mesh number of the filter screen is 10-50 mesh.
5. The process for preparing a low-density epoxy resin fracturing propping agent according to claim 1, wherein in step S8, the filtered inert medium is directly recycled to the inert medium heating tank.
6. The preparation process of the low-density epoxy resin fracturing propping agent according to claim 1, wherein the preparation system of the low-density epoxy resin fracturing propping agent comprises an epoxy resin storage tank (1), a curing agent storage tank (2), an accelerator storage tank (3), a toughening agent storage tank (4), a surface auxiliary agent storage tank (5), a batching tank (6), a resin mixed liquor temporary storage tank (7), a primary reaction kettle (8), a secondary reaction kettle (9), a tertiary reaction kettle (10), a coil pipe reactor (11) and a separating cylinder (12), wherein the epoxy resin storage tank (1) is connected with the batching tank (6) through an epoxy resin feeding pipe (15), the curing agent storage tank (2) is connected with the batching tank (6) through a curing agent feeding pipe (16), the accelerator storage tank (3) is connected with the batching tank (6) through an accelerator feeding pipe (17), the toughening agent storage tank (4) is connected with the batching tank (6) through a toughening agent feeding pipe (18), and the surface auxiliary agent storage tank (5) is connected with the batching tank (6) through a surface auxiliary agent feeding pipe (19);
The discharge port of the batching tank (6) is connected with the feed port of the resin mixed liquid temporary storage tank (7) through a conveying pipe I (20), and the resin mixed liquid temporary storage tank (7) is arranged at the rear side of a station of the batching tank (6); the feed inlet of the resin mixed liquid temporary storage tank (7) is also connected with a cold inert medium conveying pipe (21); the discharging port of the resin mixed liquid temporary storage tank (7) is connected with the feeding port of the first-stage reaction kettle (8) through a conveying pipe II (22), the first-stage reaction kettle (8) is arranged at the rear side of a station of the resin mixed liquid temporary storage tank (7), and the first-stage reaction kettle (8) is connected with a thermal inert medium conveying pipe (23); the discharge port of the primary reaction kettle (8) is connected with the feed port of the secondary reaction kettle (9) through a conveying pipe III (24), and the secondary reaction kettle (9) is arranged at the rear side of a station of the primary reaction kettle (8); the discharge port of the secondary reaction kettle (9) is connected with the feed port of the tertiary reaction kettle (10) through a conveying pipe IV (25), and the tertiary reaction kettle (10) is arranged at the rear side of a station of the secondary reaction kettle (9); the discharge port of the three-stage reaction kettle (10) is connected with the feed port of a coil reactor (11) through a conveying pipe V (2601), and the coil reactor (11) is arranged at the rear side of a station of the three-stage reaction kettle (10); the discharge port of the coil reactor (11) is connected with the feed port of the separating cylinder (12) through a conveying pipe VI (2602), and the separating cylinder (12) is arranged at the rear side of a station of the coil reactor (11); a discharge hole of the separating cylinder (12) is connected with an epoxy resin fracturing propping agent temporary storage tank;
A continuous passage for preparing the epoxy resin fracturing propping agent is formed among the material mixing tank (6), the resin mixed liquid temporary storage tank (7), the primary reaction kettle (8), the secondary reaction kettle (9), the tertiary reaction kettle (10), the coil pipe reactor (11) and the separating cylinder (12).
7. The process for preparing the low-density epoxy resin fracturing propping agent according to claim 6, wherein an inert medium outlet on the separating cylinder (12) is connected with a reflux port of the inert medium heating tank (14) through a recovery pipe (2604).
8. The process for preparing the low-density epoxy resin fracturing propping agent according to claim 1, wherein a control system of the low-density epoxy resin fracturing propping agent of the preparation process is arranged in the epoxy resin fracturing propping agent preparation system and comprises a DCS controller (26), the DCS controller (26) is connected with a human-computer interface (27) through a data input interface, the DCS controller (26) is connected with a data acquisition unit (28) through a data feedback interface, and the DCS controller (26) is connected with an execution unit (29) through a data output interface;
the DCS controller (26) comprises a batching control module (261), a pre-curing control module (262), a primary reaction control module (263), a secondary reaction control module (264), a tertiary reaction control module (265), a post-curing control module (266) and a separation control module (267);
The data acquisition unit (28) is arranged in the epoxy resin fracturing propping agent preparation system, and the data acquisition unit (28) comprises a sensor group (280) for data acquisition and transmission in the epoxy resin fracturing propping agent preparation process;
the execution unit (29) is arranged in the epoxy resin fracturing propping agent preparation system, and the execution unit (29) comprises a device group (290) for preparing and regulating the epoxy resin fracturing propping agent.
9. The process for preparing a low density epoxy fracturing proppants according to claim 8, wherein said sensor cluster (280) comprises an epoxy feed flow meter (2801), a curing agent feed flow meter (2802), an accelerator feed flow meter (2803), a toughening agent feed flow meter (2804) and a surface aid feed flow meter (2805) connected to a formulation control module (261);
the device also comprises a resin mixed liquid feeding flowmeter (2806) and a cold inert medium feeding flowmeter I (2807) which are connected with the pre-curing control module (262);
the reactor also comprises a disperse phase feeding flowmeter (2808), a thermal inert medium feeding flowmeter (2809), a primary reaction kettle temperature sensor (2810) and a primary reaction kettle pressure sensor (2811) which are connected with the primary reaction control module (263);
The device also comprises a primary reaction liquid feeding flowmeter (2812), a secondary reaction kettle temperature sensor (2813) and a secondary reaction kettle pressure sensor (2814) which are connected with the secondary reaction control module (264);
the device also comprises a secondary reaction liquid feeding flowmeter (2815), a tertiary reaction kettle temperature sensor (2816) and a tertiary reaction kettle pressure sensor (2817) which are connected with the tertiary reaction control module (265);
the device also comprises a three-stage reaction liquid feeding flowmeter (2818), a coil reactor temperature sensor (2819) and a coil reactor pressure sensor (2820) which are connected with the post-curing control module (266);
a product liquid feed flow meter (2821) connected to the separation control module (267) is also included.
10. The process for preparing the low-density epoxy resin fracturing propping agent according to claim 9, wherein the equipment group (290) comprises an epoxy resin storage tank (1), a curing agent storage tank (2), an accelerator storage tank (3), a toughening agent storage tank (4), a surface auxiliary agent storage tank (5), a batching tank (6), a resin mixed liquor temporary storage tank (7), a primary reaction kettle (8), a secondary reaction kettle (9), a tertiary reaction kettle (10), a coil pipe reactor (11) and a separation cylinder (12);
An epoxy resin feeding flowmeter (2801) is arranged on an epoxy resin feeding pipe (15) between an epoxy resin storage tank (1) and a batching tank (6), a curing agent feeding flowmeter (2802) is arranged on a curing agent feeding pipe (16) between the curing agent storage tank (2) and the batching tank (6), an accelerator feeding flowmeter (2803) is arranged on an accelerator feeding pipe (17) between the accelerator storage tank (3) and the batching tank (6), a toughening agent feeding flowmeter (2804) is arranged on a toughening agent feeding pipe (18) between a toughening agent storage tank (4) and the batching tank (6), and a surface auxiliary agent feeding flowmeter (2805) is arranged on a surface auxiliary agent feeding pipe (19) between a surface auxiliary agent storage tank (5) and the batching tank (6);
a resin mixed liquor feeding flowmeter (2806) is arranged on a conveying pipe I (20) between the batching tank (6) and the resin mixed liquor temporary storage tank (7), and a cold inert medium feeding flowmeter I (2807) is arranged on a cold inert medium conveying pipe (21) between the inert medium storage tank (13) and the resin mixed liquor temporary storage tank (7);
a disperse phase feeding flowmeter (2808) is arranged on a conveying pipe II (22) between the resin mixed liquor temporary storage tank (7) and the first-stage reaction kettle (8), a thermal inert medium feeding flowmeter (2809) is arranged on a thermal inert medium conveying pipe (23) between the inert medium heating tank (14) and the first-stage reaction kettle (8), and a first-stage reaction kettle temperature sensor (2810) and a first-stage reaction kettle pressure sensor (2811) are both arranged on the pressure of the first-stage reaction kettle (8);
A primary reaction liquid feeding flowmeter (2812) is arranged on a conveying pipe III (24) between the primary reaction kettle (8) and the secondary reaction kettle (9), and a secondary reaction kettle temperature sensor (2813) and a secondary reaction kettle pressure sensor (2814) are both arranged on the secondary reaction kettle (9);
a secondary reaction liquid feeding flowmeter (2815) is arranged on a conveying pipe IV (25) between the secondary reaction kettle (9) and the tertiary reaction kettle (10), and a tertiary reaction kettle temperature sensor (2816) and a tertiary reaction kettle pressure sensor (2817) are both arranged on the tertiary reaction kettle (10);
a three-stage reaction liquid feeding flowmeter (2818) is arranged on a conveying pipe V (2601) between the three-stage reaction kettle (10) and the coil pipe reactor (11), and a coil pipe reactor temperature sensor (2819) and a coil pipe reactor pressure sensor (2820) are both arranged on the coil pipe reactor (11);
a product liquid feeding flowmeter (2821) is arranged on a conveying pipe VI (2602) between the coil pipe reactor (11) and the separating cylinder (12).
11. The process for preparing a low density epoxy resin fracturing propping agent according to claim 10, wherein the equipment group (290) further comprises an epoxy resin regulating valve (2901) arranged on an epoxy resin feeding pipe (15), a curing agent regulating valve (2902) arranged on a curing agent feeding pipe (16), a curing agent regulating valve (2903) arranged on a curing agent feeding pipe (17), a toughening agent regulating valve (2904) arranged on a toughening agent feeding pipe (18), a surface auxiliary agent regulating valve (2917) arranged on a surface auxiliary agent feeding pipe (19), a resin mixed liquid regulating valve (2905) arranged on a conveying pipe I (20), a cold inert medium regulating valve (2906) arranged on a cold inert medium conveying pipe (21), a dispersed phase regulating valve (2907) arranged on a conveying pipe II (22), a hot inert medium regulating valve (2908) arranged on a conveying pipe III (24), a primary reaction liquid regulating valve (2909) arranged on a conveying pipe IV (25), a secondary reaction liquid regulating valve (2910) arranged on a conveying pipe VI 2911) and a product regulating valve (2602) arranged on a conveying pipe V (2602).
12. The process for preparing the low-density epoxy resin fracturing propping agent according to claim 11, wherein the equipment group (290) further comprises a batching motor (2913) arranged on the batching tank (6), a primary reaction motor (2914) arranged on the primary reaction kettle (8), a secondary reaction motor (2915) arranged on the secondary reaction kettle (9) and a tertiary reaction motor (2916) arranged on the tertiary reaction kettle (10).
13. The process for preparing the low-density epoxy resin fracturing propping agent according to claim 8, wherein the DCS controller (26) further comprises an inert medium heating control module (268), the sensor group (280) further comprises a cold inert medium feeding flowmeter ii (2822) and an inert medium heating tank temperature sensor (2823) connected with the inert medium heating control module (268), the cold inert medium feeding flowmeter ii (2822) is arranged on a pipeline between the inert medium storage tank (13) and the inert medium heating tank (14), and the inert medium heating tank temperature sensor (2823) is arranged on the inert medium heating tank (14).
14. The process for preparing the low-density epoxy resin fracturing propping agent according to claim 8, wherein the DCS controller (26) further comprises an alarm control module (269), the alarm control module (269) is connected with an alarm lamp and a loudspeaker, and the alarm lamp and the loudspeaker are distributed in the epoxy resin fracturing propping agent preparation system;
The DCS controller (26) further comprises a cleaning control module (270), wherein the cleaning control module (270) is connected with cleaning pumps, and the cleaning pumps are distributed in the epoxy resin fracturing propping agent preparation system.
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