Carbon black reaction furnace based on temperature control and optimized production preparation process

Abstract

The present application relates to the technical field of high-temperature industrial equipment manufacturing, and discloses a carbon black reaction furnace based on temperature control and an optimized production preparation process, which comprises raw material pretreatment, multi-temperature zone pyrolysis reaction, quenching termination reaction, carbon black collection and tail gas recycling. By designing a multi-temperature zone cooperative temperature control mechanism and combining with a dynamic temperature compensation technology, the uniformity and stability of the thermal field distribution in the reaction furnace are improved, the problem of uneven reaction caused by the temperature gradient of the traditional device is overcome, the carbon black nucleation and growth process are carried out in a highly controllable thermal environment, and the production of highly uniform particle size is ensured. Through the construction of online monitoring and closed-loop feedback control, real-time sensing and intelligent regulation and control of key process parameters are realized, fluctuations in the production process are timely inhibited, the reaction conditions are ensured to be always in the optimal interval, and therefore the consistency of product quality and the reliability of process operation are improved.

Description

Technical Field

[0001] This invention relates to the field of high-temperature industrial equipment manufacturing technology, specifically to a temperature-controlled carbon black reactor and an optimized production process. Background Technology

[0002] The carbon black reactor is the core equipment in the furnace carbon black production process. It consists of core components such as a combustion chamber, a throat, and a reaction chamber. Fuel and air are mixed and burned in the combustion chamber to generate a high-temperature airflow. Raw oil is injected into the reaction chamber through the throat and cracked to produce carbon black particles. By optimizing the air intake structure, fuel injection method, and waste heat recovery system, the utilization of thermal energy can be improved. Different furnace structures can control key performance indicators of carbon black such as oil absorption value, surface area, and coloring strength.

[0003] Currently, in the carbon black production process, traditional reactors generally suffer from uneven temperature field distribution and fluctuating thermal gradients, resulting in an unstable nucleation and growth environment for carbon black particles and making it difficult to achieve precise control over the particle size distribution of the product. Existing production processes lack the ability to perceive and control key parameters online in real time and in a closed-loop manner, failing to respond promptly to fluctuations in operating conditions, resulting in poor product quality consistency and large batch-to-batch differences. Insufficient coordination between units in the entire production system and low energy and raw material utilization efficiency restrict the further development of carbon black production towards high efficiency and cleanliness.

[0004] Therefore, a temperature-controlled carbon black reactor and an optimized production process are proposed to solve the above problems. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a temperature-controlled carbon black reactor and an optimized production process, which solves the problems mentioned in the background technology, such as unstable nucleation and growth environment of carbon black particles, difficulty in achieving precise control of product particle size distribution, poor product quality consistency, large batch-to-batch differences, and low energy and raw material utilization efficiency.

[0006] To achieve the above objectives, the present invention provides the following technical solution: an optimized production process for carbon black based on a temperature-controlled carbon black reactor, comprising the following steps:

[0007] Step 1: Raw material pretreatment. Liquid hydrocarbon raw materials are atomized into micron-sized particles (10-50 μm) using an atomization device and mixed with carrier gas preheated to 300-500℃ to form an aerosol.

[0008] Step Two: Multi-temperature zone pyrolysis reaction. The aerosol is introduced into a three-stage temperature-controlled reactor and passes through the following stages in sequence:

[0009] First temperature zone, preheating zone: temperature controlled at 800-900℃, residence time 0.5-1.0s;

[0010] Second temperature zone, main reaction zone: temperature controlled at 1200-1400℃, thermal field uniformity adjusted in real time by electromagnetic induction coil, temperature difference ≤±15℃, residence time 0.2-0.5s;

[0011] The third temperature zone, nucleation zone: the temperature is controlled at 1000-1100℃, and a nucleating agent solution is introduced;

[0012] Step 3: Rapid cooling to terminate the reaction. A multi-stage vortex rapid cooling device is used to cool the material to below 200℃ at a cooling rate of 200-400℃ / s.

[0013] Step 4: Carbon black collection. Solid carbon black is separated by a pulse backflush bag filter system and transported under a nitrogen protective atmosphere.

[0014] Step 5: Tail gas recycling. The reaction tail gas is treated by catalytic oxidation to remove unburned hydrocarbons and then returned to the carrier gas system.

[0015] In step two, the inner wall of the reactor is coated with a composite ceramic coating, which is composed of the following raw materials in parts by weight: 60-70 parts of silicon carbide, 15-20 parts of yttrium-stabilized zirconium oxide, and 10-15 parts of boron nitride, with a coating thickness of 200-500 μm.

[0016] The reaction temperature is dynamically adjusted based on the carbon black D50 data monitored by the online laser particle size analyzer. When the D50 deviation exceeds ±5nm, the set temperature of the three temperature zones is automatically adjusted.

[0017] Preferably, the raw material pretreatment includes:

[0018] The liquid hydrocarbon feedstock is heated to 80-120℃, atomized through an ultrasonic atomizing nozzle at a pressure of 0.5-2.0MPa, and turbulently mixed with preheated carrier gas in a mixing chamber with a swirl intensity coefficient of 1.5-3.0 for 30-60s.

[0019] Preferably, the liquid hydrocarbon feedstock is composed of the following components: 70-80 wt% coal tar, 10-15 wt% anthracene oil, and 5-10 wt% biomass pyrolysis oil, with an aromatic content ≥85% and an ash content ≤0.05%.

[0020] The nucleating agent solution is a 0.1-0.5 mol / L aqueous solution of alkali metal carbonate, and the amount injected is 0.5-1.5% of the total raw material.

[0021] Preferably, the multi-stage vortex quenching device includes three-stage cooling units:

[0022] The first stage adopts a concentric sleeve structure, with 5-10℃ cold water injected into the inner tube and -20℃ liquid nitrogen introduced into the outer tube, with a cooling rate ≥200℃ / s;

[0023] The second stage is equipped with rotating blades, with a blade tilt angle of 30-45° and a rotation speed of 500-1000 r / min;

[0024] The third stage is equipped with an ultrasonic oscillator with a frequency of 20-40kHz and a power density of 0.5-1.5W / cm².

[0025] Preferably, the exhaust gas recycling includes:

[0026] The tail gas containing CO and H2 is passed into an oxidation reactor filled with a platinum-rhodium catalyst, and the reaction temperature is controlled at 600-800℃ and the space velocity at 1000-2000 h⁻¹. -1 The CO conversion rate is ≥99%, and the treated gas is dehydrated by molecular sieve and then reused.

[0027] Temperature-controlled carbon black reactors include:

[0028] The three-stage reaction tube is made of corundum ceramic and the diameter gradually decreases from Φ200mm to Φ100mm.

[0029] The electromagnetic induction temperature control system includes three independently controlled induction coils, each covered with a three-section reaction tube, with a power density of 30-50kW / m.

[0030] A composite coating is applied to the inner wall of the reaction tube, with a surface roughness Ra≤0.2μm;

[0031] The online monitoring module includes a laser particle size analyzer and an infrared thermal imager, with a sampling frequency of 10Hz.

[0032] Preferably, the electromagnetic induction temperature control system employs a multivariable PID control algorithm, and the input variables include:

[0033] The deviation ΔT between the measured temperature and the set value in each temperature zone;

[0034] Real-time data for carbon black D50;

[0035] Rate of change in raw material flow rate;

[0036] The output variables are the current phase angle and frequency of each coil, with the current phase angle adjustable from 0 to 180° and the frequency adjustable from 5 to 20 kHz.

[0037] Preferably, the composite coating is prepared by a plasma spraying process, specifically including:

[0038] The corundum matrix was roughened by sandblasting, and the surface roughness Ra was 3.0-5.0 μm.

[0039] Silicon carbide underlayer is sprayed at a speed of 100-200 mm / s under an argon atmosphere;

[0040] Under a nitrogen atmosphere, zirconium oxide and boron nitride layers are sprayed alternately at a speed of 80-150 mm / s to form a gradient structure.

[0041] Preferably, the online monitoring module establishes a closed-loop feedback with the central controller, triggering a temperature compensation mechanism when any of the following conditions are detected:

[0042] Radial temperature difference in the main reaction zone > 20℃;

[0043] The 30-minute moving standard deviation of D50 is >3nm;

[0044] The CV value of the atomized particle size of the raw material is >15%.

[0045] Preferably, the online monitoring module includes closed-loop control logic:

[0046] When the radial temperature difference in the main reaction zone is detected to be greater than 20°C, the central controller automatically generates a temperature compensation command and adjusts the power of the electromagnetic induction coil according to the following rules:

[0047] ;

[0048] in As compensation value, It is a proportionality coefficient and its range is 0.5-1.2. The maximum radial temperature difference, Duration;

[0049] Meanwhile, when the 30-minute moving standard deviation of D50 is greater than 3nm, the pressure adjustment of the raw material atomization system is automatically triggered, and the atomized particle size CV value is reduced to below 12%.

[0050] Compared with existing technologies, this invention provides a temperature-controlled carbon black reactor and an optimized production process, which has the following advantages:

[0051] In this invention, by designing a multi-temperature zone collaborative temperature control mechanism and combining it with dynamic temperature compensation technology, the uniformity and stability of the heat field distribution in the reactor are improved, overcoming the problem of uneven reaction caused by temperature gradient in traditional devices. This allows the nucleation and growth process of carbon black to take place in a highly controllable thermal environment, ensuring the production of products with highly uniform particle size.

[0052] In this invention, by constructing online monitoring and closed-loop feedback control, real-time perception and intelligent regulation of key process parameters are achieved, fluctuations in the production process are suppressed in a timely manner, and the reaction conditions are always kept in the optimal range, thereby improving the consistency of product quality and the reliability of process operation.

[0053] In this invention, by systematically integrating and optimizing multiple process units such as efficient pretreatment of raw materials, precise control of the reaction process, rapid cooling termination, and tail gas recycling, not only is the energy and raw material utilization efficiency of the entire production process improved, but pollutant emissions are also reduced, forming a clean production process route for carbon black that is efficient, energy-saving, and environmentally friendly. Detailed Implementation

[0054] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0055] Example 1: Optimized production process of carbon black based on temperature-controlled reactor, including the following steps:

[0056] Step 1: Raw material pretreatment. Liquid hydrocarbon raw materials are atomized into micron-sized particles with a particle size of 10μm using an atomization device and mixed with carrier gas preheated to 300℃ to form an aerosol.

[0057] Step Two: Multi-temperature zone pyrolysis reaction. The aerosol is introduced into a three-stage temperature-controlled reactor and passes through the following stages in sequence:

[0058] First temperature zone, preheating zone: temperature controlled at 800℃, dwell time 0.5s;

[0059] Second temperature zone, main reaction zone: temperature controlled at 1200℃, thermal field uniformity adjusted in real time by electromagnetic induction coil, temperature difference ≤ ±15℃, residence time 0.2s;

[0060] The third temperature zone, nucleation zone: the temperature is controlled at 1000℃, and a nucleating agent solution is introduced;

[0061] Step 3: Rapid cooling to terminate the reaction. A multi-stage vortex rapid cooling device is used to cool the material to below 200°C at a cooling rate of 200°C / s.

[0062] Step 4: Carbon black collection. Solid carbon black is separated by a pulse backflush bag filter system and transported under a nitrogen protective atmosphere.

[0063] Step 5: Tail gas recycling. The reaction tail gas is treated by catalytic oxidation to remove unburned hydrocarbons and then returned to the carrier gas system.

[0064] In step two, the inner wall of the reactor is coated with a composite ceramic coating, which is composed of the following raw materials in parts by weight: 60 parts silicon carbide, 15 parts yttrium oxide-stabilized zirconium oxide, and 10 parts boron nitride, with a coating thickness of 200 μm;

[0065] The reaction temperature is dynamically adjusted based on the carbon black D50 data monitored by the online laser particle size analyzer. When the D50 deviation exceeds ±5nm, the set temperature of the three temperature zones is automatically adjusted.

[0066] Raw material pretreatment includes:

[0067] The liquid hydrocarbon feedstock is heated to 80°C, atomized through an ultrasonic atomizing nozzle at a pressure of 0.5 MPa, and turbulently mixed with preheated carrier gas in a mixing chamber with a swirl intensity coefficient of 1.5 for 30 seconds.

[0068] The liquid hydrocarbon feedstock consists of the following components: 75 wt% coal tar, 15 wt% anthracene oil, and 10 wt% biomass pyrolysis oil, with an aromatic content ≥85% and an ash content ≤0.05%.

[0069] The nucleating agent solution is a 0.1 mol / L aqueous solution of alkali metal carbonate, and the amount injected is 0.5% of the total raw material.

[0070] The multi-stage vortex quenching device includes three cooling units:

[0071] The first stage adopts a concentric sleeve structure, with 5℃ cold water injected into the inner tube and -20℃ liquid nitrogen introduced into the outer tube, with a cooling rate ≥200℃ / s;

[0072] The second stage is equipped with rotating blades, with a blade tilt angle of 30° and a rotation speed of 500 r / min;

[0073] The third stage is equipped with an ultrasonic oscillator with a frequency of 20kHz and a power density of 0.5W / cm².

[0074] Exhaust gas recycling includes:

[0075] The tail gas containing CO and H2 was passed into an oxidation reactor filled with a platinum-rhodium catalyst, and the reaction temperature was controlled at 600℃ and the space velocity at 1000 h⁻¹. -1 The CO conversion rate is ≥99%, and the treated gas is dehydrated by molecular sieve and then reused.

[0076] Temperature-controlled carbon black reactors include:

[0077] The three-stage reaction tube is made of corundum ceramic and the diameter gradually decreases from Φ200mm to Φ100mm.

[0078] The electromagnetic induction temperature control system includes three independently controlled induction coils, each covering a three-section reaction tube, with a power density of 30kW / m.

[0079] A composite coating is applied to the inner wall of the reaction tube, with a surface roughness Ra≤0.2μm;

[0080] The online monitoring module includes a laser particle size analyzer and an infrared thermal imager, with a sampling frequency of 10Hz.

[0081] The electromagnetic induction temperature control system uses a multivariable PID control algorithm, and the input variables include:

[0082] The deviation ΔT between the measured temperature and the set value in each temperature zone;

[0083] Real-time data for carbon black D50;

[0084] Rate of change in raw material flow rate;

[0085] The output variables are the current phase angle and frequency of each coil, with the current phase angle adjustable from 0 to 180° and the frequency adjustable from 5 to 20 kHz.

[0086] The composite coating is prepared by plasma spraying, specifically including:

[0087] The corundum matrix was roughened by sandblasting, and the surface roughness Ra=3.0μm;

[0088] Silicon carbide underlayer was sprayed at a speed of 100 mm / s under an argon atmosphere;

[0089] Under a nitrogen atmosphere, zirconium oxide and boron nitride layers are alternately sprayed at a speed of 80 mm / s to form a gradient structure.

[0090] The online monitoring module establishes a closed-loop feedback with the central controller, triggering a temperature compensation mechanism when any of the following conditions are detected:

[0091] Radial temperature difference in the main reaction zone > 20℃;

[0092] The 30-minute moving standard deviation of D50 is >3nm;

[0093] The CV value of the atomized particle size of the raw material is >15%.

[0094] The online monitoring module includes closed-loop control logic:

[0095] When the radial temperature difference in the main reaction zone is detected to be greater than 20°C, the central controller automatically generates a temperature compensation command and adjusts the power of the electromagnetic induction coil according to the following rules:

[0096] ;

[0097] in As compensation value, It is a proportionality coefficient and its range is 0.5-1.2. The maximum radial temperature difference, Duration;

[0098] Meanwhile, when the 30-minute moving standard deviation of D50 is greater than 3nm, the pressure adjustment of the raw material atomization system is automatically triggered, and the atomized particle size CV value is reduced to below 12%.

[0099] Example 2: Optimized production process of carbon black based on temperature-controlled reactor, including the following steps:

[0100] Step 1: Raw material pretreatment. Liquid hydrocarbon raw materials are atomized into micron-sized particles with a particle size of 30μm using an atomization device and mixed with carrier gas preheated to 400℃ to form an aerosol.

[0101] Step Two: Multi-temperature zone pyrolysis reaction. The aerosol is introduced into a three-stage temperature-controlled reactor and passes through the following stages in sequence:

[0102] First temperature zone, preheating zone: temperature controlled at 850℃, dwell time 0.85s;

[0103] Second temperature zone, main reaction zone: temperature controlled at 1300℃, thermal field uniformity adjusted in real time by electromagnetic induction coil, temperature difference ≤ ±15℃, residence time 0.35s;

[0104] Third temperature zone, nucleation zone: temperature controlled at 1050℃, nucleating agent solution is introduced;

[0105] Step 3: Rapid cooling to terminate the reaction. A multi-stage vortex rapid cooling device is used to cool the material to below 200°C at a cooling rate of 300°C / s.

[0106] Step 4: Carbon black collection. Solid carbon black is separated by a pulse backflush bag filter system and transported under a nitrogen protective atmosphere.

[0107] Step 5: Tail gas recycling. The reaction tail gas is treated by catalytic oxidation to remove unburned hydrocarbons and then returned to the carrier gas system.

[0108] In step two, the inner wall of the reactor is coated with a composite ceramic coating, which is composed of the following raw materials in parts by weight: 65 parts silicon carbide, 18 parts yttrium oxide-stabilized zirconium oxide, and 13 parts boron nitride, with a coating thickness of 350 μm;

[0109] The reaction temperature is dynamically adjusted based on the carbon black D50 data monitored by the online laser particle size analyzer. When the D50 deviation exceeds ±5nm, the set temperature of the three temperature zones is automatically adjusted.

[0110] Raw material pretreatment includes:

[0111] The liquid hydrocarbon feedstock is heated to 100°C, atomized through an ultrasonic atomizing nozzle at a pressure of 1.3 MPa, and turbulently mixed with preheated carrier gas in a mixing chamber with a swirl intensity coefficient of 2.3 for 45 seconds.

[0112] The liquid hydrocarbon feedstock consists of the following components: 80 wt% coal tar, 10 wt% anthracene oil, and 10 wt% biomass pyrolysis oil, with an aromatic content ≥85% and an ash content ≤0.05%.

[0113] The nucleating agent solution is a 0.3 mol / L aqueous solution of alkali metal carbonate, and the amount injected is 1.0% of the total raw material.

[0114] The multi-stage vortex quenching device includes three cooling units:

[0115] The first stage adopts a concentric sleeve structure, with 8℃ cold water injected into the inner tube and -20℃ liquid nitrogen introduced into the outer tube, with a cooling rate ≥200℃ / s;

[0116] The second stage is equipped with rotating blades, with a blade tilt angle of 38° and a rotation speed of 750 r / min;

[0117] The third stage is equipped with an ultrasonic oscillator with a frequency of 30kHz and a power density of 1.0W / cm².

[0118] Exhaust gas recycling includes:

[0119] The tail gas containing CO and H2 was passed into an oxidation reactor filled with a platinum-rhodium catalyst, and the reaction temperature was controlled at 700℃ and the space velocity at 1500 h⁻¹. -1 The CO conversion rate is ≥99%, and the treated gas is dehydrated by molecular sieve and then reused.

[0120] Temperature-controlled carbon black reactors include:

[0121] The three-stage reaction tube is made of corundum ceramic and the diameter gradually decreases from Φ200mm to Φ100mm.

[0122] The electromagnetic induction temperature control system includes three independently controlled induction coils, each covered with a three-section reaction tube, with a power density of 40kW / m.

[0123] A composite coating is applied to the inner wall of the reaction tube, with a surface roughness Ra≤0.2μm;

[0124] The online monitoring module includes a laser particle size analyzer and an infrared thermal imager, with a sampling frequency of 10Hz.

[0125] The electromagnetic induction temperature control system uses a multivariable PID control algorithm, and the input variables include:

[0126] The deviation ΔT between the measured temperature and the set value in each temperature zone;

[0127] Real-time data for carbon black D50;

[0128] Rate of change in raw material flow rate;

[0129] The output variables are the current phase angle and frequency of each coil, with the current phase angle adjustable from 0 to 180° and the frequency adjustable from 5 to 20 kHz.

[0130] The composite coating is prepared by plasma spraying, specifically including:

[0131] The corundum matrix was roughened by sandblasting, and the surface roughness Ra=4.0μm;

[0132] Silicon carbide underlayer was sprayed at a speed of 150 mm / s under an argon atmosphere;

[0133] Under a nitrogen atmosphere, zirconium oxide and boron nitride layers are alternately sprayed at a speed of 115 mm / s to form a gradient structure.

[0134] The online monitoring module establishes a closed-loop feedback with the central controller, triggering a temperature compensation mechanism when any of the following conditions are detected:

[0135] Radial temperature difference in the main reaction zone > 20℃;

[0136] The 30-minute moving standard deviation of D50 is >3nm;

[0137] The CV value of the atomized particle size of the raw material is >15%.

[0138] The online monitoring module includes closed-loop control logic:

[0139] When the radial temperature difference in the main reaction zone is detected to be greater than 20°C, the central controller automatically generates a temperature compensation command and adjusts the power of the electromagnetic induction coil according to the following rules:

[0140] ;

[0141] in As compensation value, It is a proportionality coefficient and its range is 0.5-1.2. The maximum radial temperature difference, Duration;

[0142] Meanwhile, when the 30-minute moving standard deviation of D50 is greater than 3nm, the pressure adjustment of the raw material atomization system is automatically triggered, and the atomized particle size CV value is reduced to below 12%.

[0143] Example 3: Optimized production process of carbon black based on temperature-controlled reactor, including the following steps:

[0144] Step 1: Raw material pretreatment. Liquid hydrocarbon raw materials are atomized into micron-sized particles with a particle size of 50μm using an atomization device and mixed with carrier gas preheated to 500℃ to form an aerosol.

[0145] Step Two: Multi-temperature zone pyrolysis reaction. The aerosol is introduced into a three-stage temperature-controlled reactor and passes through the following stages in sequence:

[0146] First temperature zone, preheating zone: temperature controlled at 900℃, dwell time 1.0s;

[0147] Second temperature zone, main reaction zone: temperature controlled at 1400℃, thermal field uniformity adjusted in real time by electromagnetic induction coil, temperature difference ≤ ±15℃, residence time 0.5s;

[0148] Third temperature zone, nucleation zone: temperature controlled at 1100℃, nucleating agent solution is introduced;

[0149] Step 3: Rapid cooling to terminate the reaction. A multi-stage vortex rapid cooling device is used to cool the material to below 200°C at a cooling rate of 400°C / s.

[0150] Step 4: Carbon black collection. Solid carbon black is separated by a pulse backflush bag filter system and transported under a nitrogen protective atmosphere.

[0151] Step 5: Tail gas recycling. The reaction tail gas is treated by catalytic oxidation to remove unburned hydrocarbons and then returned to the carrier gas system.

[0152] In step two, the inner wall of the reactor is coated with a composite ceramic coating, which is composed of the following raw materials in parts by weight: 70 parts silicon carbide, 20 parts yttrium-stabilized zirconium oxide, and 15 parts boron nitride, with a coating thickness of 500 μm;

[0153] The reaction temperature is dynamically adjusted based on the carbon black D50 data monitored by the online laser particle size analyzer. When the D50 deviation exceeds ±5nm, the set temperature of the three temperature zones is automatically adjusted.

[0154] Raw material pretreatment includes:

[0155] The liquid hydrocarbon feedstock is heated to 120°C, atomized through an ultrasonic atomizing nozzle at a pressure of 2.0 MPa, and turbulently mixed with preheated carrier gas in a mixing chamber at a swirl intensity coefficient of 3.0 for 60 seconds.

[0156] The liquid hydrocarbon feedstock consists of the following components: 80 wt% coal tar, 15 wt% anthracene oil, and 5 wt% biomass pyrolysis oil, with an aromatic content ≥85% and ash content ≤0.05%.

[0157] The nucleating agent solution is a 0.5 mol / L aqueous solution of alkali metal carbonate, and the amount injected is 1.5% of the total raw material.

[0158] The multi-stage vortex quenching device includes three cooling units:

[0159] The first stage adopts a concentric sleeve structure, with 10℃ cold water injected into the inner tube and -20℃ liquid nitrogen introduced into the outer tube, with a cooling rate ≥200℃ / s;

[0160] The second stage is equipped with rotating blades, with a blade tilt angle of 45° and a rotation speed of 1000 r / min;

[0161] The third stage is equipped with an ultrasonic oscillator with a frequency of 40kHz and a power density of 1.5W / cm².

[0162] Exhaust gas recycling includes:

[0163] The tail gas containing CO and H2 was passed into an oxidation reactor filled with a platinum-rhodium catalyst, and the reaction temperature was controlled at 800℃ and the space velocity at 2000 h⁻¹. -1 The CO conversion rate is ≥99%, and the treated gas is dehydrated by molecular sieve and then reused.

[0164] Temperature-controlled carbon black reactors include:

[0165] The three-stage reaction tube is made of corundum ceramic and the diameter gradually decreases from Φ200mm to Φ100mm.

[0166] The electromagnetic induction temperature control system includes three independently controlled induction coils, each covered with a three-section reaction tube, with a power density of 50kW / m.

[0167] A composite coating is applied to the inner wall of the reaction tube, with a surface roughness Ra≤0.2μm;

[0168] The online monitoring module includes a laser particle size analyzer and an infrared thermal imager, with a sampling frequency of 10Hz.

[0169] The electromagnetic induction temperature control system uses a multivariable PID control algorithm, and the input variables include:

[0170] The deviation ΔT between the measured temperature and the set value in each temperature zone;

[0171] Real-time data for carbon black D50;

[0172] Rate of change in raw material flow rate;

[0173] The output variables are the current phase angle and frequency of each coil, with the current phase angle adjustable from 0 to 180° and the frequency adjustable from 5 to 20 kHz.

[0174] The composite coating is prepared by plasma spraying, specifically including:

[0175] The corundum matrix was roughened by sandblasting, and the surface roughness Ra=5.0μm;

[0176] Silicon carbide underlayer was sprayed at a speed of 200 mm / s under an argon atmosphere;

[0177] Under a nitrogen atmosphere, zirconium oxide and boron nitride layers are sprayed alternately at a speed of 150 mm / s to form a gradient structure.

[0178] The online monitoring module establishes a closed-loop feedback with the central controller, triggering a temperature compensation mechanism when any of the following conditions are detected:

[0179] Radial temperature difference in the main reaction zone > 20℃;

[0180] The 30-minute moving standard deviation of D50 is >3nm;

[0181] The CV value of the atomized particle size of the raw material is >15%.

[0182] The online monitoring module includes closed-loop control logic:

[0183] When the radial temperature difference in the main reaction zone is detected to be greater than 20°C, the central controller automatically generates a temperature compensation command and adjusts the power of the electromagnetic induction coil according to the following rules:

[0184] ;

[0185] in As compensation value, It is a proportionality coefficient and its range is 0.5-1.2. The maximum radial temperature difference, Duration;

[0186] Meanwhile, when the 30-minute moving standard deviation of D50 is greater than 3nm, the pressure adjustment of the raw material atomization system is automatically triggered, and the atomized particle size CV value is reduced to below 12%.

[0187] Comparative Example 1: The difference between this comparative example and Example 1 is that this comparative example does not use electromagnetic induction dynamic temperature control technology in the main reaction zone of the reactor, but instead uses the traditional fixed power heating method.

[0188] Comparative Example 2 differs from Example 1 in that: this comparative example does not have online monitoring and closed-loop feedback control, and the adjustment of process parameters relies on manual experience.

[0189] Comparative Example 3 differs from Example 1 in that it does not use a three-stage vortex quenching device, but instead uses a traditional single-stage water-cooling quenching method.

[0190] Comparative Example 4 differs from Example 1 in that the reaction tail gas was not subjected to catalytic oxidation treatment and recycling, and the tail gas was directly emitted.

[0191] The carbon black products prepared in Examples 1-3 and Comparative Examples 1-4 were subjected to performance tests. The test items and test methods are as follows:

[0192] Particle size distribution was tested using laser diffraction and a particle size analyzer to measure the median particle size D50.

[0193] Structural property testing was conducted using the dibutyl phthalate absorbance method, employing an absorber to determine the degree of carbon black structural development.

[0194] Surface chemical properties were tested using the iodine adsorption method, and the surface activity of carbon black was determined using an automated iodine value analyzer.

[0195] Dispersibility test: The sieve residue determination method was used, and a 325-mesh standard sieve was used to determine the coarse particle content in the carbon black product.

[0196] The test data of the carbon black products prepared in Examples 1-3 and Comparative Examples 1-4 are recorded in the table below:

[0197]

[0198] By comparing and analyzing the data in the table, it can be seen that the carbon black products prepared using processes 1-3 have significantly better performance than those prepared using processes 1-4. This indicates that the present invention, through the design of a multi-temperature zone collaborative temperature control mechanism combined with dynamic temperature compensation technology, improves the uniformity and stability of the heat field distribution within the reactor, overcomes the problem of uneven reaction caused by temperature gradients in traditional devices, and allows the carbon black nucleation and growth process to take place in a highly controllable thermal environment, ensuring the production of products with highly uniform particle size. By constructing online monitoring and closed-loop feedback control, real-time perception and intelligent regulation of key process parameters are achieved, timely suppression of fluctuations in the production process, and ensuring that the reaction conditions are always within the optimal range, thereby improving the consistency of product quality and the reliability of process operation. By systematically integrating and optimizing multiple process units such as efficient raw material pretreatment, precise control of the reaction process, rapid cooling termination, and tail gas recycling, not only is the energy and raw material utilization efficiency of the entire production process improved, but pollutant emissions are also reduced, forming a highly efficient, energy-saving, and environmentally friendly clean production process route for carbon black.

[0199] By comparing and analyzing the relevant data in the table, it can be seen that the carbon black product produced by the preparation process of this invention has excellent particle size uniformity, structural regularity and surface activity.

[0200] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0201] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. An optimized production process for carbon black based on a temperature-controlled reactor, characterized by: Includes the following steps: Step 1: Raw material pretreatment. Liquid hydrocarbon raw materials are atomized into micron-sized particles (10-50 μm) using an atomization device and mixed with carrier gas preheated to 300-500℃ to form an aerosol. Step Two: Multi-temperature zone pyrolysis reaction. The aerosol is introduced into a three-stage temperature-controlled reactor and passes through the following stages in sequence: First temperature zone, preheating zone: temperature controlled at 800-900℃, residence time 0.5-1.0s; Second temperature zone, main reaction zone: temperature controlled at 1200-1400℃, thermal field uniformity adjusted in real time by electromagnetic induction coil, temperature difference ≤±15℃, residence time 0.2-0.5s; The third temperature zone, nucleation zone: the temperature is controlled at 1000-1100℃, and a nucleating agent solution is introduced; Step 3: Rapid cooling to terminate the reaction. A multi-stage vortex rapid cooling device is used to cool the material to below 200℃ at a cooling rate of 200-400℃ / s. Step 4: Carbon black collection. Solid carbon black is separated by a pulse backflush bag filter system and transported under a nitrogen protective atmosphere. Step 5: Tail gas recycling. The reaction tail gas is treated by catalytic oxidation to remove unburned hydrocarbons and then returned to the carrier gas system. In step two, the inner wall of the reactor is coated with a composite ceramic coating, which is composed of the following raw materials in parts by weight: 60-70 parts of silicon carbide, 15-20 parts of yttrium-stabilized zirconium oxide, and 10-15 parts of boron nitride, with a coating thickness of 200-500 μm. The reaction temperature is dynamically adjusted based on the carbon black D50 data monitored by the online laser particle size analyzer. When the D50 deviation exceeds ±5nm, the set temperature of the three temperature zones is automatically adjusted. The reactor includes an online monitoring module: The online monitoring module establishes a closed-loop feedback with the central controller, triggering a temperature compensation mechanism when any of the following conditions are detected: Radial temperature difference in the main reaction zone > 20℃, 30-minute standard deviation of D50 > 3nm, and CV value of atomized raw material > 15%; The online monitoring module includes closed-loop control logic: When the radial temperature difference in the main reaction zone is detected to be greater than 20°C, the central controller automatically generates a temperature compensation command and adjusts the power of the electromagnetic induction coil according to the following rules: ； in This is the power compensation value. It is a proportionality coefficient and its range is 0.5-1.

2. The maximum radial temperature difference, Duration; Meanwhile, when the 30-minute moving standard deviation of D50 is greater than 3nm, the pressure adjustment of the raw material atomization system is automatically triggered, and the atomized particle size CV value is reduced to below 12%.

2. The optimized production process of carbon black based on temperature control in a carbon black reactor according to claim 1, characterized in that: The raw material pretreatment includes: The liquid hydrocarbon feedstock is heated to 80-120℃, atomized through an ultrasonic atomizing nozzle at a pressure of 0.5-2.0MPa, and turbulently mixed with preheated carrier gas in a mixing chamber with a swirl intensity coefficient of 1.5-3.0 for 30-60s.

3. The optimized production process of carbon black based on temperature control in a carbon black reactor according to claim 1, characterized in that: The liquid hydrocarbon feedstock is composed of the following components: 70-80 wt% coal tar, 10-15 wt% anthracene oil, and 5-10 wt% biomass pyrolysis oil, with an aromatic content ≥85% and ash content ≤0.05%. The nucleating agent solution is a 0.1-0.5 mol / L aqueous solution of alkali metal carbonate, and the amount injected is 0.5-1.5% of the total raw material.

4. The optimized production process of carbon black reactor based on temperature control according to claim 1, characterized in that: The multi-stage vortex rapid cooling device includes three cooling units: The first stage adopts a concentric sleeve structure, with 5-10℃ cold water injected into the inner tube and -20℃ liquid nitrogen introduced into the outer tube, with a cooling rate ≥200℃ / s; The second stage is equipped with rotating blades, with a blade tilt angle of 30-45° and a rotation speed of 500-1000 r / min; The third stage is equipped with an ultrasonic oscillator with a frequency of 20-40kHz and a power density of 0.5-1.5W / cm².

5. The optimized production process of carbon black based on temperature control in a carbon black reactor according to claim 1, characterized in that: The exhaust gas recycling includes: The tail gas containing CO and H2 is passed into an oxidation reactor filled with a platinum-rhodium catalyst, and the reaction temperature is controlled at 600-800℃ and the space velocity at 1000-2000 h⁻¹. -1 The CO conversion rate is ≥99%, and the treated gas is dehydrated by molecular sieve and then reused.

6. A temperature-controlled carbon black reactor, used to implement the optimized production process of the temperature-controlled carbon black reactor as described in any one of claims 1-5, characterized in that: include: The three-stage reaction tube is made of corundum ceramic and the diameter gradually decreases from Φ200mm to Φ100mm. The electromagnetic induction temperature control system includes three independently controlled induction coils, each covered with a three-section reaction tube, with a power density of 30-50kW / m. The electromagnetic induction temperature control system adopts a multivariable PID control algorithm. The input variables include the deviation ΔT between the measured temperature and the set value of each temperature zone, the real-time data of carbon black D50, and the raw material flow rate change rate. The output variables are the current phase angle and frequency of each coil, wherein the current phase angle adjustment range is 0-180° and the frequency adjustment range is 5-20kHz. A composite coating is applied to the inner wall of the reaction tube, with a surface roughness Ra≤0.2μm; The online monitoring module includes a laser particle size analyzer and an infrared thermal imager, with a sampling frequency of 10Hz; The online monitoring module establishes a closed-loop feedback with the central controller. When the radial temperature difference in the main reaction zone is >20℃, the 30-minute moving standard deviation of D50 is >3nm, or the CV value of the raw material atomized particle size is >15%, the temperature compensation mechanism is triggered. The online monitoring module includes closed-loop control logic: When the radial temperature difference in the main reaction zone is detected to be greater than 20℃, the central controller automatically generates a temperature compensation command and adjusts the power of the electromagnetic induction coil. The adjustment rule is as follows: ； in This is the power compensation value. It is a proportionality coefficient and its range is 0.5-1.

2. The maximum radial temperature difference, Duration; Meanwhile, when the 30-minute moving standard deviation of D50 is greater than 3nm, the pressure adjustment of the raw material atomization system is automatically triggered, so that the atomized particle size CV value is reduced to below 12%.

7. The temperature-controlled carbon black reactor according to claim 6, characterized in that: The composite coating is prepared by plasma spraying, specifically including: The corundum matrix was roughened by sandblasting, and the surface roughness Ra was 3.0-5.0 μm. Silicon carbide underlayer is sprayed at a speed of 100-200 mm / s under an argon atmosphere; Under a nitrogen atmosphere, zirconium oxide and boron nitride layers are sprayed alternately at a speed of 80-150 mm / s to form a gradient structure.

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