Continuous kettle type reaction rectification production device of high temperature emulsifier for oil base drilling fluid
Patent Information
- Application Number
- CN202521857573.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-29
- Publication Date
- 2026-09-18
- Estimated Expiration
- 2035-08-29
AI Technical Summary
然而,该间歇法存在以下固有缺陷:1)因反应釜需反复加热和冷却,导致能量效率低下;2)间歇反应和蒸馏操作反应产物品质操作周期较长,反应和蒸馏温度随时间波动难以控制,导致反应速率和蒸馏效率不稳定,产品质量批次差异大;3)间歇反应和蒸馏操作需要完成一个完整的间歇操作流程:检漏、进料、蒸馏、卸料、清洗,需要大量的人力和物力,过多的操作带来较大安全隐患;4)高温操作加剧设备损耗和物料分解风险
[0015]This invention relates to a continuous, closed-loop reaction-separation cycle system for producing high-temperature emulsifiers for oil-based drilling fluids. The system integrates a reactor and distillation column, and introduces an azeotropic organic carrier that reacts with water. The basic principle is to utilize azeotropic distillation to continuously "carry" the water generated in the reaction zone (high temperature, high viscosity) as a low-boiling-point azeotrope, disrupting the reaction equilibrium and forcing the reaction to continue towards the product phase. The separated carrier is then returned to the reaction zone for reuse. The entire process is conducted under slight negative pressure to lower the boiling point, and precise temperature control is achieved through an external circulating heating/cooling system. Multi-layer stirring ensures material uniformity, and a high-efficiency packed tower and phase separation tank ensure effective separation. Ultimately, this system achieves efficient, energy-saving, stable, and continuous production of high-quality high-temperature emulsifiers under relatively mild conditions.
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Abstract
Description
Technical Field
[0001] This utility model relates to the field of high-temperature emulsifier preparation technology for oil-based drilling fluids, specifically to a continuous batch reaction distillation production device for high-temperature emulsifiers for oil-based drilling fluids. Background Technology
[0002] In oil drilling operations, the high-temperature stability of oil-based drilling fluids is crucial, and their performance depends on highly efficient high-temperature emulsifiers. These high-temperature emulsifiers (such as polyamides, polyethers, and siloxanes) need to maintain their activity under high temperature and pressure conditions to significantly reduce oil-water interfacial tension and form stable emulsions. However, the synthesis process of such high-temperature emulsifiers faces many challenges: high reaction temperatures, high system viscosity, and difficulty in removing byproducts (water), resulting in long production cycles, high energy consumption, low product yields, and large quality fluctuations.
[0003] Traditional processes for producing high-temperature emulsifiers generally employ batch operation: the reactants are fed into a reactor all at once, heated to the reaction temperature (e.g., 170°C) via a jacket (using steam or heat transfer oil) and held at that temperature for an extended period, during which some byproducts are distilled off; after the reaction, the temperature is raised again (e.g., to 250°C) for deep distillation to remove residual byproducts. However, this batch method has the following inherent drawbacks: 1) The reactor requires repeated heating and cooling, resulting in low energy efficiency; 2) The batch reaction and distillation operations have long operating cycles, and the reaction and distillation temperatures fluctuate over time, making it difficult to control, leading to unstable reaction rates and distillation efficiency, and significant batch-to-batch variations in product quality; 3) Batch reaction and distillation operations require a complete batch operation process: leak detection, feeding, distillation, unloading, and cleaning, requiring substantial manpower and resources, and excessive operations pose significant safety hazards; 4) High-temperature operation exacerbates equipment wear and the risk of material decomposition. Utility Model Content
[0004] In order to achieve continuous, stable, efficient and low-energy production of high-temperature emulsifiers for oil-based drilling fluids, this utility model proposes an uninterrupted batch reaction distillation production device for high-temperature emulsifiers for oil-based drilling fluids.
[0005] The present invention relates to an uninterrupted batch-type reactive distillation production apparatus for high-temperature emulsifiers for oil-based drilling fluids, comprising: a reactor, a distillation column, a condenser, a phase-separated reflux tank, a phase-separated water storage tank, a circulating heating pump, an external heating system for the reactor, an external cooling system for the reactor, a circulating cooling pump, and a production pump; wherein, the gas phase outlet at the top of the reactor is connected to the inlet at the bottom of the distillation column; the gas phase outlet at the top of the distillation column is connected to the hot-side inlet of the condenser; the liquid phase outlet of the condenser is connected to the phase-separated reflux tank; the oil phase outlet of the phase-separated reflux tank is connected to the reflux port at the top of the distillation column via a reflux pipeline, and the water phase outlet of the phase-separated reflux tank is connected to the phase-separated water storage tank; the outer wall of the reactor is covered with a jacket, which forms a heating circulation loop with the external heating system via the circulating heating pump, and the reactor also forms a cooling circulation loop with the external cooling system via the circulating cooling pump; the discharge port at the bottom of the reactor is connected to the downstream storage tank via the production pump.
[0006] Furthermore, the uninterrupted batch reaction distillation production unit for high-temperature emulsifiers for oil-based drilling fluids also includes a vacuum system connected to the gas phase outlet of the condenser.
[0007] Furthermore, the reactor is equipped with at least two layers of stirring paddles.
[0008] Furthermore, each layer of agitators is connected to a drive motor located outside the reactor via an independent drive shaft.
[0009] Furthermore, the distillation column is equipped with a structured packing layer, which is composed of multiple layers of thin sheets stacked together, with multiple airflow holes on the sheets.
[0010] Furthermore, a trough-type liquid distributor is provided above the structured packing layer, and multiple distribution holes are uniformly opened on the trough-type liquid distributor.
[0011] Furthermore, a vertical baffle is provided inside the phase-separated reflux tank. The top of the vertical baffle is sealed to the top of the phase-separated reflux tank, and a gap is provided between the bottom of the vertical baffle and the bottom of the phase-separated reflux tank.
[0012] Furthermore, the spacing should not exceed one-quarter of the height of the phase-separated reflux tank.
[0013] Furthermore, the reactor has a feed inlet formed on its sidewall, which is used to simultaneously feed in the raw material of the high-temperature emulsifier for oil-based drilling fluid and the water carrier.
[0014] Furthermore, the water carrier is selected from one of toluene, xylene, butyl acetate, isoamyl acetate, butyl ether, ethylene glycol monobutyl ether, cyclohexane, and methylcyclohexane.
[0015] This invention relates to a continuous, closed-loop reaction-separation cycle system for producing high-temperature emulsifiers for oil-based drilling fluids. The system integrates a reactor and distillation column, and introduces an azeotropic organic carrier that reacts with water. The basic principle is to utilize azeotropic distillation to continuously "carry" the water generated in the reaction zone (high temperature, high viscosity) as a low-boiling-point azeotrope, disrupting the reaction equilibrium and forcing the reaction to continue towards the product phase. The separated carrier is then returned to the reaction zone for reuse. The entire process is conducted under slight negative pressure to lower the boiling point, and precise temperature control is achieved through an external circulating heating / cooling system. Multi-layer stirring ensures material uniformity, and a high-efficiency packed tower and phase separation tank ensure effective separation. Ultimately, this system achieves efficient, energy-saving, stable, and continuous production of high-quality high-temperature emulsifiers under relatively mild conditions.
[0016] Compared with existing intermittent high-temperature production methods, the uninterrupted batch reactive distillation production device for high-temperature emulsifiers for oil-based drilling fluids of this invention adopts reactive distillation coupling technology and introduces an azeotropic carrier circulation system, successfully reducing the reaction temperature from 250℃ in the traditional process to about 110℃. This not only significantly reduces energy consumption and equipment requirements, but also greatly improves the reaction conversion rate and product yield by continuously removing external product water, ensuring the stability of product quality. At the same time, the continuous and automated operation of the entire process overcomes the inherent disadvantages of intermittent production, such as long production cycles, cumbersome operation, high labor costs, and high safety risks, forming an innovative solution for high-efficiency, energy-saving, environmentally friendly, and easily scaled-up industrial production of high-temperature emulsifiers. Attached Figure Description
[0017] Figure 1 This is a schematic diagram of the uninterrupted batch reaction distillation production apparatus for high-temperature emulsifiers for oil-based drilling fluids according to an embodiment of the present invention. Detailed Implementation
[0018] To better understand the purpose, structure, and function of this utility model, a more detailed description of this utility model is provided below with reference to the accompanying drawings.
[0019] Figure 1 The structure of a continuous batch-type reactive distillation production apparatus 100 for high-temperature emulsifiers for oil-based drilling fluids according to an embodiment of the present invention is shown. Figure 1As shown, the uninterrupted batch reaction distillation production device 100 for high-temperature emulsifiers for oil-based drilling fluids may include: a reactor 1, a distillation column 2, a condenser 3, a phase-separated reflux tank 4, a phase-separated water storage tank 5, a circulating heating pump 6, an external heating system for the reactor 7, an external cooling system for the reactor 8, a circulating cooling pump, and a production pump 14. The gas phase outlet at the top of reactor 1 is connected to the inlet at the bottom of distillation column 2; the gas phase outlet at the top of distillation column 2 is connected to the hot side inlet of condenser 3; the liquid phase outlet of condenser 3 is connected to phase-separated reflux tank 4; the oil phase outlet of phase-separated reflux tank 4 is connected to the reflux port at the top of distillation column 2 through reflux pipeline 42; the water phase outlet of phase-separated reflux tank 4 is connected to phase-separated water storage tank 5; the outer wall of reactor 1 is covered with a jacket 10, which forms a heating circulation loop with external heating system 7 via circulating heating pump 6; reactor 1 also forms a cooling circulation loop with external cooling system 8 via circulating cooling pump; the discharge port at the bottom of reactor 1 is connected to downstream storage tank 15 via discharge pump 14.
[0020] In operation, the uninterrupted batch reaction distillation production apparatus 100 for high-temperature emulsifiers for oil-based drilling fluids of this utility model allows the reactant 16 and water carrier (described in detail below) to be fed into the reactor 1 through the feed inlet. The external heating system 7 is activated (the heating temperature is preferably maintained at 90-280°C), and the heat medium heats the reactor 1 via the jacket 10, initiating a reaction within the reactor 1 and generating water. The operating pressure within the reactor 1 is preferably 70-90 kPaA, and the reaction temperature is preferably maintained at 90-280°C. Water and the carrier form an azeotropic vapor, which continuously enters the distillation column 2 from the top of the reactor 1 in vapor form. The operating pressure within the distillation column 2 is preferably 70-90 kPaA, the bottom temperature is preferably maintained at 90-280°C, and the top temperature is preferably maintained at 80-110°C. Inside the distillation column 2, the vapor is purified and then liquefied in the condenser 3. The condensate flows into the phase-separated reflux tank 4 for settling and stratification. The upper oil phase (rich in carrier) is refluxed back to the distillation column 2 to continue the cycle, while the lower aqueous phase is discharged to the phase-separated water storage tank 5, thus achieving continuous water removal. The operating pressure of the condenser 3 and the phase-separated reflux tank 4 is preferably 70-90 kPa, and the material temperature is preferably maintained at 40-60°C. After the reaction is complete, the product is pumped out via the collection pump 14. If necessary, the external cooling system 8 can be switched to rapidly cool the material to prevent changes in physical properties after dehydration. The circulating liquid temperature can be maintained at 40-140°C as needed. After the production cycle is completed, the water carrier can be stored in the distillation column 2, condenser 3, and phase-separated reflux tank 4 for use in the next production cycle without loss.
[0021] The uninterrupted batch reaction distillation production device 100 for high-temperature emulsifiers for oil-based drilling fluids in this embodiment of the present invention constructs a complete continuous reaction distillation production system. By integrating the reactor 1 with equipment such as the distillation column 2, condenser 3, and phase separation reflux tank 4, the reaction and separation are carried out simultaneously. The external circulation temperature control system enables precise, rapid, and flexible control of the reaction temperature, significantly shortening the production cycle. The addition of distillation column 2 increases the separation precision of reaction byproducts (such as water) and the target product, effectively removing byproducts and improving reaction conversion. The reflux operation of the water carrier in distillation column 2 further achieves high-precision separation between byproducts and reaction products, preventing product loss during distillation and improving yield. The coupled reactive distillation and azeotropic dehydration mechanism (utilizing the azeotropic properties of the water carrier to significantly lower the boiling point of water) allows the reaction and dehydration processes to proceed efficiently at temperatures far below the normal boiling point of water, enabling continuous online removal of byproducts, breaking reaction equilibrium limitations, and thus significantly improving reaction conversion and product yield while ensuring product quality stability. The entire unit achieves continuous and integrated operation of reaction and separation, providing a fundamental guarantee for the efficient, continuous, and stable production of high-temperature emulsifiers.
[0022] According to this utility model, in such Figure 1 In the preferred embodiment shown, the uninterrupted batch reactive distillation production apparatus 100 for high-temperature emulsifiers for oil-based drilling fluids may further include a vacuum system 9, which is connected to the gas phase outlet of the condenser 3. By adding the vacuum system 9, the operating pressure (preferably 70-90 kPaA) in the reactor 1 and distillation column 2 can be maintained at a slightly negative pressure (preferably 60-90 kPaA), enabling azeotropic dehydration to be achieved at a lower temperature. This significantly reduces the operating temperature of the reaction system (e.g., from 250°C in the original process to 110°C), thereby greatly reducing energy consumption, reducing the risk of decomposition of heat-sensitive materials, and simultaneously enhancing the dehydration effect and improving the reaction conversion rate.
[0023] In such Figure 1 In the preferred embodiment shown, reactor 1 may be equipped with at least two layers of stirring paddles 11. This arrangement enhances the mixing and mass and heat transfer efficiency of high-viscosity materials within reactor 1, ensuring uniform temperature of the reactants, thorough reaction, avoiding localized overheating or reaction dead zones, and improving reaction rate and product consistency. It should be noted that the addition of the aforementioned water-carrying agent also reduces the viscosity of the high-viscosity materials within reactor 1, thereby reducing the power consumption required for stirring and accelerating the reaction rate.
[0024] Preferably, each layer of stirring paddles 11 can be connected to a drive motor 13 located outside the reactor 1 via an independent drive shaft 12. Each layer of stirring paddles 11 is driven independently, and the speed can be adjusted independently according to the viscosity of different materials and the requirements of the reaction stage, realizing more flexible and precise stirring control, and further optimizing the mixing effect and energy consumption.
[0025] According to this utility model, in such Figure 1 In the preferred embodiment shown, the distillation column 2 may be provided with a structured packing layer 21, which may be composed of multiple layers of thin sheets stacked together. The thin sheets have multiple gas flow holes, so that the structured packing layer 21 has a complex regular flow channel. This complex regular flow channel helps to provide a larger and more ordered mass transfer surface for the gas and liquid phases, while maintaining an extremely low system pressure drop, thereby achieving high separation efficiency under high throughput, which perfectly matches the energy-saving requirements of vacuum operation.
[0026] In a preferred embodiment, these sheets can be rolled into a corrugated shape, with the angle and height of the corrugations precisely designed. The sheets can be perforated, rolled with fine lines or punctured to promote uniform distribution of liquid on the surface (film formation) and enhance surface wettability, while gas can also pass through these small holes to increase the gas-liquid contact area.
[0027] Preferably, the material of the sheet can be selected from metal, plastic, and ceramic. Further, the metal can be stainless steel, carbon steel, titanium, Monel alloy, etc., and the plastic can be PP, PVDF, etc.
[0028] In such Figure 1 In the preferred embodiment shown, a trough-type liquid distributor 22 may be provided above the structured packing layer 21, and the trough-type liquid distributor 22 may have multiple distribution holes evenly formed on it. The diameter of the distribution holes is preferably 1-3 mm. The structured packing layer 21 combined with the liquid distributor 22 improves the separation efficiency and processing capacity of the distillation column 2, ensures sufficient contact between the gas and liquid phases, and ensures uniform distribution of the reflux liquid.
[0029] In such Figure 1 In the preferred embodiment shown, a vertical baffle 41 may be provided inside the phase-separating reflux tank 4. The top of the vertical baffle 41 is sealed to the top of the phase-separating reflux tank 4, and a gap is provided between the bottom of the vertical baffle 41 and the bottom of the phase-separating reflux tank 4. The vertical baffle 41 is used to buffer the liquid flowing into the phase-separating reflux tank 4, stabilize the liquid surface, reduce disturbance, create a stable separation environment for the oil and water phases, effectively promote the stratification of the two phases, prevent mutual entrainment, and ensure the purity of the carrier and the dehydration effect.
[0030] Preferably, the spacing is no greater than one-quarter of the height of the phase separation reflux tank 4. This design optimizes the hydrodynamic state of the separation chamber, ensuring optimal separation buffering effect and phase separation interface stability, and is an effective design parameter proven in practice.
[0031] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this utility model, and not to limit it. Although this utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. These modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this utility model, and they should all be covered within the scope of the claims and specification of this utility model. In particular, as long as there is no structural conflict, the various technical features mentioned in the embodiments can be combined in any way. This utility model is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.
Claims
1. An uninterrupted kettle reaction rectification production device of high temperature emulsifier for oil-based drilling fluid, characterized in that, include: The reactor comprises a distillation column, a condenser, a phase-separated reflux tank, a phase-separated water storage tank, a circulating heating pump, an external heating system for the reactor, an external cooling system for the reactor, a circulating cooling pump, and a product pump. The vapor outlet at the top of the reactor is connected to the inlet at the bottom of the distillation column. The vapor outlet at the top of the distillation column is connected to the hot-side inlet of the condenser. The liquid outlet of the condenser is connected to the phase-separated reflux tank. The oil outlet of the phase-separated reflux tank is connected to the reflux port at the top of the distillation column via a reflux pipeline. The water outlet of the phase-separated reflux tank is connected to the phase-separated water storage tank. The outer wall of the reactor is covered with a jacket, which forms a heating circulation loop with the external heating system via the circulating heating pump. The reactor also forms a cooling circulation loop with the external cooling system via the circulating cooling pump. The outlet at the bottom of the reactor is connected to a downstream storage tank via the product pump.
2. The uninterrupted kettle reaction rectification production apparatus for high-temperature emulsifiers for oil-based drilling fluids according to claim 1, characterized in that, The uninterrupted batch reaction distillation production unit for high-temperature emulsifiers for oil-based drilling fluids also includes a vacuum system, which is connected to the gas phase outlet of the condenser.
3. The uninterrupted kettle reaction rectification production apparatus for high-temperature emulsifiers for oil-based drilling fluids according to claim 1 or 2, characterized in that, The reactor is equipped with at least two layers of stirring paddles.
4. The uninterrupted kettle reaction rectification production apparatus for high-temperature emulsifiers for oil-based drilling fluids according to claim 3, characterized in that, Each layer of the stirring paddle is connected to a drive motor located outside the reactor via an independent drive shaft.
5. The uninterrupted kettle reaction rectification production apparatus for high-temperature emulsifiers for oil-based drilling fluids according to claim 1 or 2, characterized in that, The distillation column is equipped with a structured packing layer, which is composed of multiple layers of thin sheets stacked together, and the thin sheets have multiple airflow holes.
6. The uninterrupted kettle reaction rectification production apparatus for high-temperature emulsifiers for oil-based drilling fluids according to claim 5, characterized in that, A trough-type liquid distributor is provided above the structured packing layer, and the trough-type liquid distributor has multiple distribution holes evenly distributed on it.
7. The uninterrupted kettle reaction rectification production apparatus for high-temperature emulsifiers for oil-based drilling fluids according to claim 1 or 2, characterized in that, The phase-separating reflux tank is equipped with a vertical partition. The top of the vertical partition is sealed to the top of the phase-separating reflux tank, and a gap is provided between the bottom of the vertical partition and the bottom of the phase-separating reflux tank.
8. The uninterrupted kettle reaction rectification production apparatus for high-temperature emulsifiers for oil-based drilling fluids according to claim 7, characterized in that, The spacing is no greater than one-quarter of the height of the phase-separated reflux tank.
9. The uninterrupted kettle reaction rectification production apparatus for high-temperature emulsifiers for oil-based drilling fluids according to claim 1 or 2, characterized in that, The reactor has a feed inlet formed on its side wall, which is used to simultaneously feed in the raw material of the high-temperature emulsifier for oil-based drilling fluid and the water carrier.
10. The uninterrupted kettle reaction rectification production apparatus for high-temperature emulsifiers for oil-based drilling fluids according to claim 9, characterized in that, The water carrier is selected from one of toluene, xylene, butyl acetate, isoamyl acetate, butyl ether, ethylene glycol monobutyl ether, cyclohexane, and methylcyclohexane.