Centrifugal extraction and purification device for chemical production

Abstract

The invention discloses a centrifugal extraction and purification device for chemical production, and particularly relates to the technical field of chemical production, the centrifugal extraction and purification device comprises a modular multi-stage extraction unit which is composed of at least two centrifugal extractors connected in series, a spiral mixed flow deflector and a separation weir plate are arranged in each extractor drum, and counter-current extraction is supported; and the intelligent control system integrates a flow sensor, an online turbidity analyzer and an AI algorithm module. According to the invention, the mixing-separation integrated rotary drum is adopted and is internally divided into a mixing section and a separation section, a mass transfer path is shortened by virtue of an adjustable transition channel, mixing is enhanced by virtue of a micron-sized groove, and emulsification is inhibited by virtue of an electrochromic variable-viscosity coating; a magnetic suspension bearing replaces a traditional bearing and is matched with a vibration suppressor to prolong the service life of equipment; operating parameters are optimized by applying a deep reinforcement learning model, and energy consumption and solvent consumption are reduced; the multi-stage series connection reduces the inter-stage pressure drop, the special material and the coating enable the device to resist strong acid and alkali corrosion, the defects of traditional equipment are effectively overcome, and the performance is greatly improved in multiple aspects.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical production, and particularly relates to a centrifugal extraction and purification device for chemical production. Background Art

[0002] In chemical production, it is often necessary to separate and purify various mixtures to obtain high-purity target products. As an efficient separation method, the centrifugal extraction and purification technology has been widely used in the chemical field. The centrifugal extraction and purification device came into being under such a background. It uses a centrifugal force field to strengthen the extraction process, enabling the rapid separation of two-phase liquids under the action of centrifugal force; Traditional equipment mostly adopts a fixed diversion structure or a single stirring impeller, resulting in insufficient mixing intensity or too long mixing time, leading to low mass transfer efficiency. Traditional mechanical bearings and shaft seal structures are prone to wear during high-speed operation, resulting in frequent shutdowns for maintenance. The vibration generated during high-speed rotation is likely to cause fatigue damage to the equipment. Traditional shock absorption structures rely on springs or damping fluids, with limited suppression efficiency, and it is difficult to effectively control the resonance frequency band (50 - 200 Hz), affecting the stability of the separation interface. Traditional equipment parameter adjustment relies on manual experience and cannot dynamically respond to changes in material properties (such as viscosity, pH), resulting in high solvent loss and large purity fluctuations. Summary of the Invention

[0003] The purpose of the present invention is to provide a centrifugal extraction and purification device for chemical production to solve the above-mentioned deficiencies in the technology.

[0004] To achieve the above purpose, the present invention provides the following technical solution: A centrifugal extraction and purification device for chemical production, comprising: A modular multi-stage extraction unit: composed of at least two centrifugal extractors connected in series, with spiral mixing diversion vanes and separation weir plates arranged inside the drum of each extractor to support countercurrent extraction; An intelligent control system: integrated with a flow sensor, an on-line turbidity analyzer, and an AI algorithm module to real-time monitor the two-phase flow ratio, interface position, and separation effect, and dynamically adjust the rotation speed, flow rate, and weir plate height; A self-balancing shock absorption structure: a magnetic levitation bearing and a piezoelectric vibration suppressor are arranged between the drum and the drive shaft to achieve automatic correction of dynamic balance; A two-phase sequential feeding system: including a heavy-phase storage tank, a light-phase storage tank, and a preheating module, and controlling the injection of the two phases into the drum in a preset order (first the heavy phase and then the light phase) through a proportional valve; A mixing-separation integrated drum: the inner cavity of the drum is divided into an upper mixing section (equipped with a turbine impeller) and a lower separation section (equipped with a conical disc stack), and the mixing section and the separation section are connected through an adjustable transition channel.

[0005] Preferably, in the modular multi-stage extraction unit, adjacent centrifugal extractors are connected by a detachable sealed pipeline, and a Venturi effect accelerator is arranged inside the pipeline to reduce the inter-stage transmission pressure drop.

[0006] Preferably, the AI algorithm module of the intelligent control system is based on a deep reinforcement learning model, predicts the optimal speed-flow matching curve according to historical operation data, and generates dynamic adjustment instructions.

[0007] Preferably, an electro-responsive variable viscosity coating is installed in the transition channel of the mixing-separation integrated drum, and the surface hydrophilicity and hydrophobicity of the coating are changed by applying a voltage to actively control the position of the two-phase interface.

[0008] Preferably, the piezoelectric vibration suppressor of the self-balancing shock absorption structure is linked with the strain sensor on the outer wall of the drum. When the detected vibration frequency > 50 Hz, the reverse damping force compensation is automatically triggered.

[0009] Preferably, the preheating module of the two-phase sequential feeding system uses microwave-assisted heating, and the heating power is linearly correlated with the feeding flow rate to ensure that the temperature difference between the two-phase liquids ≤ 2 °C.

[0010] Preferably, the drum material is carbon fiber reinforced polyether ether ketone (CF / PEEK), and the surface is coated with a titanium nitride (TiN) wear-resistant coating, which is suitable for strong acid (pH < 2) or strong base (pH > 12) environments.

[0011] In the above technical solutions, the technical effects and advantages provided by the present invention are as follows: 1. Through the design of the mixing-separation integrated drum, the inside of the drum is divided into a mixing section (turbine impeller) and a separation section (conical disc stack), which are connected by an adjustable transition channel, shortening the mass transfer path. The micron-scale grooves on the surface of the spiral guide vane enhance turbulent mixing, reducing the mixing time from 20 seconds to 8 seconds, and the mass transfer coefficient is increased to 1.8×10⁻ 4 m / s16. Combining with the active control of the interface position by the electro-responsive variable viscosity coating, the diffusion of the emulsion layer is effectively inhibited.

[0012] 2. Using magnetic levitation bearings to replace traditional mechanical bearings, eliminating frictional losses, and cooperating with piezoelectric vibration suppressors to offset high-frequency vibrations (> 50 Hz) in real time, with the vibration amplitude controlled within < 5 μm, and the equipment life extended to more than 12,000 hours 3. Dynamically optimizing the speed, flow rate and weir plate height based on the deep reinforcement learning model, and the reward function comprehensively considering purity, energy consumption and solvent saving rate, reducing the unit processing energy consumption by 35% and the solvent consumption by 28%.

[0013] 4. The multi - stage series connection reduces the pressure drop between stages (0.3 MPa → 0.1 MPa) through a Venturi - effect accelerator. The CF / PEEK drum matrix and TiN coating can withstand strong acids (pH < 2) or strong alkalis (pH > 12), with an annual corrosion rate < 0.01 mm, solving the corrosion defects of traditional stainless steel or titanium materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required in the embodiments. Obviously, the drawings described below are only some embodiments recorded in the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings.

[0015] Figure 1 It is a schematic diagram of the overall structure of the present invention; Figure 2 It is a schematic diagram of the connection structure of the centrifugal extractor and the on - line turbidity analyzer of the present invention; Figure 3 It is a schematic diagram of the connection structure of the centrifugal extractor and the magnetic levitation bearing of the present invention; Figure 4 It is a schematic diagram of the sectional structure of the present invention; Figure 5 It is a schematic diagram of the step - by - step process of the present invention.

[0016] Description of the reference numerals in the drawings: 1. Centrifugal extractor; 2. Separation weir plate; 3. Flow sensor; 4. On - line turbidity analyzer; 5. Magnetic levitation bearing; 6. Piezoelectric vibration suppressor; 7. Heavy - phase storage tank; 8. Light - phase storage tank; 9. Pre - heating module. SPECIFIC EMBODIMENTS

[0017] In order to enable those skilled in the art to better understand the technical solutions of the present invention, the following will further introduce the present invention in detail in conjunction with the drawings.

[0018] The present invention provides a centrifugal extraction and purification device for chemical production as shown in Figures 1 to 5 and includes: 1.1 Modular multi - stage extraction unit Structural composition: Inside the drum (diameter 300 - 1500 mm) of each centrifugal extractor, there are spiral mixing guide vanes (the adjustable range of the pitch is 10 - 50 mm, and the guide angle is 15° - 45°). The surface of the guide vanes is covered with a micron - level groove structure (depth 0.1 - 0.5 mm) for enhancing the turbulent mixing of the two - phase fluid; Separation weir plate design: The height of the weir plate is driven by a servo motor (adjustment accuracy ±0.1 mm). A double-channel overflow weir is set at the outlet of the separation section (the light-phase outlet is located at the top of the drum, and the heavy-phase outlet is located at the bottom). The material of the weir plate is silicon carbide ceramic (hardness ≥2800 HV); Realization of countercurrent extraction: Adjacent drums are connected by a diversion pipe inclined at 30°. The heavy-phase liquid flows from the heavy-phase outlet of the upper stage into the light-phase inlet of the lower stage, and the light phase flows in the opposite direction to form a countercurrent mass transfer gradient.

[0019] 1.2 Intelligent control system Sensor configuration: An electromagnetic flowmeter (accuracy ±0.5% FS) is installed in the two-phase feed pipeline to monitor the flow rate in real time (range 0 - 1000 L / h); An on-line turbidity analyzer (wavelength 860 nm, detection range 0 - 1000 NTU) is embedded at the outlet of the separation section, and the clarity data of the separation interface is obtained through an optical fiber probe; AI algorithm module: Deployed on an embedded industrial computer (computing power ≥4 TOPS), using a deep reinforcement learning framework (the state space includes rotational speed, flow rate, and turbidity; the action space is the rotational speed adjustment amount and the weir plate displacement amount), and an adjustment instruction is generated every 10 seconds.

[0020] 1.3 Self-balancing shock absorption structure Magnetic suspension bearing: The radial clearance is 50 - 100 μm. The eccentricity displacement of the drum is monitored by a Hall sensor (resolution 0.1 μm), and the current of the electromagnetic coil is adjusted through a PID controller (response time <1 ms); Piezoelectric vibration suppressor: Piezoelectric ceramic sheets (PZT-5H type) are attached to the outer wall of the drum. After the vibration signal is analyzed by FFT, an anti-phase damping waveform is generated (frequency range 10 - 1000 Hz, suppression efficiency ≥90%).

[0021] 1.4 Dual-phase sequential feeding system Proportional valve control logic: The outlet valve of the heavy-phase storage tank (diameter DN50) is opened first. After the flow rate stabilizes to the set value (fluctuation <±2%), the outlet valve of the light-phase storage tank (diameter DN40) is opened with a delay of 5 - 30 seconds; Preheating module: Adopts double spiral coils (material 316L stainless steel). The heavy-phase pipeline is wound with a heating tape (power density 2 W / cm²), and the light-phase pipeline uses a microwave resonator (frequency 2.45 GHz, power adjustable from 0 - 5 kW).

[0022] 1.5 Mixing-separation integrated drum Mixing section design: The turbine impeller (diameter accounting for 60% of the inner diameter of the drum) is composed of 6 arc-shaped blades (inclination angle 25°, thickness 3 mm), with a rotational speed range of 500 - 6000 rpm, generating a local shear rate >1000 s⁻¹; Separation section design: The surface of the conical disc stack (cone angle 40°, layer spacing 1.5 mm) is sprayed with a hydrophobic modified coating (contact angle > 120°) to accelerate the aggregation of the light phase (organic phase) towards the center; Adjustable transition channel: The channel width is controlled by a hydraulic actuator (adjustment range 5 - 20 mm), and the inner wall of the channel is provided with flow guiding ribs (height 2 mm, spacing 10 mm) to suppress eddy currents.

[0023] 2. Venturi effect accelerator The ratio of the throat diameter of the Venturi tube to the diameter of the inter-stage pipeline is 1:3, the flow velocity at the throat is increased to 3 - 5 m / s, and the inter-stage pressure drop is reduced from 0.3 MPa in the traditional design to below 0.1 MPa; A wear-resistant bushing (made of tungsten carbide, hardness ≥ 2000 HV) is embedded in the throat to prevent erosion and wear by high-solid-content materials.

[0024] 3. Deep reinforcement learning model Training data source: Historical operation database (including 10 5 sets of rotational speed - flow rate - turbidity correlation data), and the reward function is set as R = k1 ⋅ purity + k2 ⋅ solvent saving rate - k3 ⋅ energy consumption (coefficients k1 = 0.6, k2 = 0.3, k3 = 0.1); Model output: Generate a fitting formula for the rotational speed - flow rate matching curve (a, b are dynamic correction coefficients, n is the rotational speed, Q is the flow rate).

[0025] 4. Electro-responsive viscosity coating Coating material: Polyaniline / graphene composite material (thickness 50 - 200 μm), when a voltage of 0 - 10 V is applied, the surface contact angle changes from 30° (hydrophilic) to 150° (superhydrophobic); Control logic: When the entrainment amount of the light phase is detected > 1%, apply an 8 V voltage to the coating to lower the interface position by 3 - 5 mm and reduce entrainment.

[0026] 5. Vibration suppression linkage mechanism Strain sensor: Patch-type resistance strain gauge (sensitivity coefficient 2.0), arranged at 0°, 120°, and 240° azimuths on the outer wall of the drum; Reverse damping force compensation: The piezoelectric ceramic sheet outputs a peak voltage of ±200 V with a phase difference of 180°, effectively suppressing the resonance frequency band (50 - 200 Hz).

[0027] 6. Microwave-assisted heating Microwave resonator design: Rectangular TE 10Mode cavity (size 245mm×122mm×80mm), the material flows through a polytetrafluoroethylene (PTFE) conduit (diameter 25mm), voltage standing wave ratio ≤ 1.5; Temperature control: The power of the magnetron (0 - 5kW) is adjusted by the PID algorithm to make the temperature difference between the two-phase liquid ≤ 2°C (the accuracy of the thermocouple is ±0.1°C).

[0028] 7. Composite coating on the drum Substrate material: Carbon fiber reinforced polyether ether ketone (CF / PEEK, fiber volume fraction 40%, tensile strength ≥ 300MPa); Surface treatment: Physical vapor deposition (PVD) titanium nitride coating (thickness 3 - 5μm, microhardness ≥ 2200HV), resistant to corrosion by 10% HCl or 30% NaOH solution (annual corrosion rate < 0.01mm).

[0029] Example 1: Structure assembly and operation of the intelligent multi-stage centrifugal extraction and purification device 1. Device assembly Modular multi-stage extraction unit: Three centrifugal extractors (drum diameter 800mm) are connected in series through detachable sealed pipes, and a Venturi effect accelerator (throat diameter 25mm, bushing material is tungsten carbide) is installed inside the pipes; Mixed-separation integrated drum: Spiral mixing guide vanes (pitch 30mm, guide angle 30°) and a conical disc group (layer spacing 1.5mm) are assembled inside the drum, and the width of the transition channel is preset to 12mm; Self-balancing shock absorption structure: Magnetic suspension bearings (radial clearance 80μm) and piezoelectric vibration suppressors (PZT-5H type ceramic chips, covering 60% of the outer wall area of the drum) are installed.

[0030] Intelligent control system: An electromagnetic flowmeter (range 0 - 800L / h) is deployed in the feed pipe, and an on-line turbidity analyzer (detection accuracy ±1NTU) is installed at the outlet of the separation section. The industrial control computer is pre-installed with a deep reinforcement learning algorithm model.

[0031] 2. Operating procedure Step 1: Material preheating and feeding The heavy phase (phenol-containing wastewater, density 1.2g / cm³) is heated to 50°C (power 3kW) through the microwave resonant cavity, and the light phase (methyl isobutyl ketone, density 0.8 g / cm³) is heated to 48°C through the electric heating tape. The temperature difference between the two phases is controlled within 2°C; According to the preset program, the heavy-phase proportional valve (flow rate 300L / h) is opened first, and after the flow rate is stable, the light-phase proportional valve (flow rate 200L / h) is opened after a 15-second delay.

[0032] Step 2: Setting of mixing and separation parameters The initial rotational speed is set at 3500 rpm, and the AI algorithm generates a rotational speed - flow rate curve based on historical data. , and the height of the weir plate is dynamically adjusted to 10.2 mm; A 5V voltage is applied to the electro - responsive viscosity coating to adjust the contact angle of the transition channel surface to 110°, optimizing the two - phase interface position.

[0033] Step 3: Multi - stage counter - current extraction The heavy phase enters the second - stage light - phase inlet through a deflector tube inclined at 30° from the first - stage heavy - phase outlet, and the light phase flows in the opposite direction, forming a three - stage counter - current extraction; The Venturi accelerator reduces the inter - stage transfer pressure drop from 0.25 MPa to 0.08 MPa to ensure flow balance.

[0034] Step 4: Dynamic feedback regulation When the turbidity analyzer detects that the entrainment amount of the second - stage light phase reaches 1.5%, the AI model immediately increases the rotational speed to 4200 rpm, lowers the height of the weir plate to 9.8 mm, and applies an 8V voltage to the electro - responsive coating simultaneously; When the vibration suppressor detects a resonance peak at 65 Hz, it triggers a reverse damping waveform (phase difference 180°, voltage ± 150V), and the vibration amplitude decreases from 15 μm to 2 μm.

[0035] 3. Operating effects Extraction efficiency: The recovery rate of phenolic compounds is increased from 82% in single - stage extraction to 98.5%, and the solvent consumption is reduced by 28%; Energy consumption data: The unit processing energy consumption is 0.85 kWh / m³, which is 32% lower than that of traditional equipment; Stability test: After continuous operation for 72 hours, there is no sign of corrosion on the drum coating (in an environment with pH = 1.5), and the turbidity monitoring error is stable within ± 1.5%.

[0036] Example 2: Application of high - efficiency purification of pharmaceutical intermediates Application scenario Purify the naproxen sodium intermediate (the aqueous phase contains the target product, and the organic phase is ethyl acetate), with a processing capacity of 500 L / h.

[0037] 2. Key configuration adjustments The drum material is replaced with a CF / PEEK matrix + TiN coating (resistant to 30% NaOH corrosion); The microwave pre - heating power is adjusted to 4 kW, and the temperatures of the two phases are synchronized to 40 ± 0.5 °C; The reward function coefficients of the AI model are adjusted to k1 = 0.7, k2 = 0.25, k3 = 0.05, with an emphasis on optimizing the product purity.

[0038] 3. Operating results Purity improvement: The purity of the target product is increased from 89.3% to 99.1%, and the entrainment amount of the organic phase is <0.3%; Vibration control: At a rotational speed of 6000 rpm, the vibration amplitude of the drum is maintained at ≤3 μm, and the bearing temperature is stabilized at 45°C; Maintenance cycle: After continuous operation for 6000 hours, the wear amount of the Venturi bushing is <0.1 mm, and there is no need to stop the machine for replacement.

[0039] Example 3: Verification of adaptability to high-viscosity materials Test object Polymer solution (viscosity 1200 mPa·s, aqueous phase) - n-heptane (organic phase) system, throughput 200 L / h.

[0040] 2. Special configuration The modular unit is extended to 5-stage series connection, and the diameter of the Venturi throat is increased to 40 mm; The width of the transition channel is adjusted to 18 mm, and the voltage of the electrocoating is increased to 10 V (contact angle 150°); The deep reinforcement learning model introduces the viscosity sensor data, and the rotation speed formula is updated to .

[0041] 3. Performance data Mass transfer enhancement: The mixing time is shortened to 6 seconds, and the mass transfer coefficient reaches 2.1×10⁻ 4 m / s; Pressure drop control: The total pressure drop of the five-stage series connection is only 0.4 MPa (traditional design ≥1.2 MPa); Thermal management: Microwave heating makes the temperature uniformity of the high-viscosity aqueous phase (standard deviation ≤0.3°C), avoiding local overheating and degradation.

[0042] Summary of example effects Efficiency breakthrough: Three-stage countercurrent extraction makes the recovery rate of the target substance generally >98%, and the mass transfer efficiency is increased by 40-60%; Intelligent adaptability: The AI algorithm dynamically responds to changes in material properties (such as viscosity, pH), and the adjustment accuracy is 5 times higher than that of the traditional PID control; Reliability under extreme conditions: Under complex conditions such as strong corrosion, high vibration, and high viscosity, the continuous operation life of the device exceeds 10,000 hours.

[0043] Synergy of modularization and intelligent control The Venturi accelerator (claim 2) reduces the inter-stage pressure drop, enabling the AI algorithm (claim 3) to flexibly distribute the flow rate of each stage during multi-stage series connection, avoiding flow imbalance caused by pressure loss.

[0044] Dynamic interface regulation and shock absorption linkage The electro-viscous coating (Claim 4) actively adjusts the interface position, combined with vibration suppression (Claim 5), to ensure the stability of the separation interface at high speeds (>4000 rpm) and avoid the diffusion of the emulsion layer.

[0045] Compatibility of materials with heating The low coefficient of thermal expansion (3×10⁻ 6 / °C) of the CF / PEEK drum (Claim 7) matches the rapid temperature rise characteristics of microwave heating (Claim 6), preventing thermal stress cracking.

[0046] Only some exemplary embodiments of the present invention have been described above by way of illustration. Undoubtedly, for those of ordinary skill in the art, the described embodiments can be modified in various different ways without departing from the spirit and scope of the present invention. Therefore, the above drawings and description are illustrative in nature and should not be construed as limiting the scope of the claims of the present invention.

Claims

1. A centrifugal extraction and purification device for chemical production, characterized in that, Including: Modular multi-stage extraction unit: Composed of at least two centrifugal extractors connected in series. Each extractor drum is equipped with spiral mixing guide vanes and a separation weir plate to support countercurrent extraction; Intelligent control system: Integrated with a flow sensor, an on-line turbidity analyzer, and an AI algorithm module to monitor the two-phase flow ratio, interface position, and separation effect in real time, and dynamically adjust the rotation speed, flow rate, and weir plate height; Self-balancing shock absorption structure: A magnetic levitation bearing and a piezoelectric vibration suppressor are arranged between the drum and the drive shaft to achieve automatic correction of dynamic balance; Dual-phase sequential feeding system: Comprising a heavy-phase storage tank, a light-phase storage tank, and a preheating module. The two phases are injected into the drum in a preset order (heavy phase first and then light phase) through a proportional valve; Integrated mixing-separation drum: The inner cavity of the drum is divided into an upper mixing section (equipped with a turbine impeller) and a lower separation section (equipped with a conical disc stack). The mixing section and the separation section are connected by an adjustable transition channel.

2. The centrifugal extraction and purification device for chemical production according to claim 1, wherein: In the modular multi-stage extraction unit, adjacent centrifugal extractors are connected by a detachable sealed pipeline, and a Venturi effect accelerator is arranged inside the pipeline to reduce the inter-stage transfer pressure drop.

3. A centrifugal extraction and purification device for chemical production according to claim 1, characterized in that: The AI algorithm module of the intelligent control system is based on a deep reinforcement learning model, predicts the optimal rotation speed-flow rate matching curve according to historical operation data, and generates dynamic adjustment instructions.

4. A centrifugal extraction and purification device for chemical production according to claim 1, characterized in that: An electro-responsive variable viscosity coating is installed in the transition channel of the integrated mixing-separation drum. By applying a voltage, the surface hydrophilicity and hydrophobicity of the coating are changed to achieve active control of the two-phase interface position.

5. A centrifugal extraction and purification device for chemical production according to claim 1, characterized in that: The piezoelectric vibration suppressor of the self-balancing shock absorption structure is linked with a strain sensor on the outer wall of the drum. When the detected vibration frequency > 50 Hz, a reverse damping force compensation is automatically triggered.

6. The centrifugal extraction and purification device for chemical production according to claim 1, characterized in that: The preheating module of the dual-phase sequential feeding system uses microwave-assisted heating, and the heating power is linearly correlated with the feeding flow rate to ensure that the temperature difference between the two-phase liquids ≤ 2°C.

7. A centrifugal extraction and purification device for chemical production according to claim 1, characterized in that: The drum material is carbon fiber reinforced polyether ether ketone (CF / PEEK), and the surface is coated with a titanium nitride (TiN) wear-resistant coating, which is suitable for strong acid (pH < 2) or strong base (pH > 12) environments.

Images