Special reaction kettle for naphthenic modification of naphthyl aromatic hydrocarbon

By using a multi-order heating ring, vortex nozzle and dynamic stirring system in the reactor, the limitations of traditional reactors in raw material dispersion, temperature control and stirring mass transfer are solved, and efficient chemical reactions are achieved, and the purity and yield of the product are improved.

CN120205067APending Publication Date: 2025-06-27ZHONGKAI UNIV OF AGRI & ENG
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Patent Information

Application Number
CN202510349980.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-24
Publication Date
2025-06-27

AI Technical Summary

Technical Problem

Traditional reactors have limitations in raw material dispersion, temperature control and stirred mass transfer, resulting in insufficient reactions, increased side reactions, low product purity and yield, making it difficult to meet the demand for narrow molecular weight distribution in high-end applications.

Method used

A special reactor was designed, using a multi-step heating ring, vortex nozzle and a dynamic stirring system to achieve gradient temperature control and efficient dispersion of raw materials, and enhance stirring strength and mass transfer efficiency.

Benefits of technology

By accurately adjusting the temperature and efficiently dispersing raw materials, side reactions are suppressed, the purity and yield of the product are improved, and the demand for narrow molecular weight distribution in high-end applications is met.

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Abstract

The invention discloses a special reaction kettle for naphthyl arene naphthenic modification, and relates to the technical field of chemical production, the special reaction kettle comprises a reaction kettle body, a stirring motor is arranged at the top of the reaction kettle body, a stirring rod is arranged at the output end of the stirring motor, the stirring rod extends into the reaction kettle body, and two groups of stirring paddles are arranged on the stirring rod; a plurality of stages of heating rings are arranged on the outer wall of the reaction kettle and are independently arranged. According to the synergistic regulation reaction kettle for naphthyl aromatic hydrocarbon naphthenation modification, the dispersity is improved through the multi-stage vortex nozzles, the molecular weight is precisely regulated and controlled in combination with gradient temperature control and a dynamic stirring system, and the synergistic regulation reaction kettle is suitable for industrial production of high-performance lubricating oil and high polymer material additives.
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Description

Technical Field

[0001] The present invention relates to the technical field of chemical production, and in particular to a special reaction kettle for the cyclization modification of naphthyl aromatic hydrocarbons. Background Art

[0002] In the fields of chemical production and the like, the reaction kettle, as a key device for carrying out chemical reactions, its reaction efficiency and product quality are affected by various factors. Traditional reaction kettles have certain limitations in aspects such as raw material dispersion, temperature control, and stirring mass transfer. For example, uneven dispersion of raw materials leads to incomplete reactions, local overheating causes side reactions and reduces product purity, and low stirring efficiency prolongs the reaction time. The cyclization reaction of naphthyl aromatic hydrocarbons (such as polycyclic aromatic hydrocarbons like naphthalene and anthracene) is a key step in the preparation of high-performance lubricants, polymer material additives, and pharmaceutical intermediates. Traditional reaction kettles mostly adopt single-layer stirring and straight-tube nozzle designs, and have the following defects:

[0003] Insufficient dispersion: Traditional nozzles cannot achieve efficient dispersion of raw materials, resulting in insufficient contact between reactants and an increase in side reactions. Wide molecular weight distribution: During the reaction process, the temperature fluctuates greatly (±5°C), it is difficult to precisely control the degree of polycondensation, and the molecular weight distribution range of the product is wide (usually 300 - 800 Da), which is difficult to meet the requirements of high-end applications for a narrow molecular weight distribution (such as ±50 Da). Limited process conditions: Existing reaction kettles have weak ability to synergistically regulate the ratio, temperature, and time, and it is difficult to achieve precise molecular weight regulation through single-parameter adjustment. Therefore, there is an urgent need for a new type of reaction kettle that can synergistically regulate reaction conditions and improve product uniformity. Summary of the Invention

[0004] The purpose of the present invention is to solve the defects existing in the prior art, and to propose a special reaction kettle for the cyclization modification of naphthyl aromatic hydrocarbons.

[0005] In order to achieve the above purpose, the present invention adopts the following technical solutions:

[0006] A special reaction kettle for the cyclization modification of naphthyl aromatic hydrocarbons, including a reaction kettle body, a stirring motor is arranged at the top of the reaction kettle body, a stirring rod is arranged at the output end of the stirring motor, the stirring rod extends into the reaction kettle body, and two groups of stirring paddles are arranged on the stirring rod; a multi-stage heating ring is arranged on the outer wall of the reaction kettle, and multiple heating rings are independently arranged.

[0007] Furthermore, an inlet is arranged at the top of the reaction kettle, an opening and closing cover is arranged at the inlet, and a knob is arranged on the opening and closing cover, and the knob is used to control the opening and closing of the opening and closing cover.

[0008] Further, a vortex nozzle is provided at the top of the reactor. The vortex nozzle includes an upper inclined nozzle and a lower inclined nozzle. There are 4 - 6 groups of upper inclined nozzles, and conical spiral guide vanes are arranged inside the upper inclined nozzles; there are 4 - 6 groups of lower inclined nozzles; and conical spiral guide vanes are arranged inside the lower inclined nozzles.

[0009] Further, the two sets of stirring paddles on the stirring rod are respectively an inclined blade paddle and an anchor paddle. The anchor paddle is arranged below the inclined blade paddle. There are 4 - 6 groups of inclined blade paddles, and the blade inclination angle is 30 - 60°.

[0010] Further, three groups of heating rings are provided, which are respectively arranged in the upper, middle, and lower layers of the reactor body. A heat conduction tube is arranged inside the heating ring. The heat conduction tube is connected to an external heat supply source, and a temperature control component is arranged on the heat conduction tube.

[0011] Further, at least three temperature detectors are arranged inside the reactor body. The three temperature detectors are arranged on the stirring shaft and are respectively arranged corresponding to each layer of heating ring.

[0012] Further, the material of the reactor body is Hastelloy, and the wall thickness is 20 mm.

[0013] Beneficial Effects

[0014] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0015] The gradient temperature control system can accurately adjust the temperature according to the temperature requirements at different stages and positions of the chemical reaction, effectively suppressing side reactions caused by local overheating. Compared with the traditional overall temperature control reactor, the gradient temperature control system can better meet the special requirements of complex chemical reactions for temperature distribution, improving the purity and yield of the product.

[0016] The multi - stage vortex nozzle is installed on the feed pipeline of the reactor. Compared with the traditional direct - injection nozzle, the combined action of the spiral structure and the Venturi effect of the multi - stage vortex nozzle can more effectively disperse the raw materials into tiny droplets, avoiding the agglomeration phenomenon of the raw materials in the reactor and providing more favorable conditions for subsequent chemical reactions.

[0017] The inclined blade paddle can generate strong axial and radial flows, fully mixing the materials and pushing the materials to circulate in the reactor. The anchor paddle is close to the bottom of the reactor body, which can effectively prevent the materials from depositing at the bottom and enhance the exchange of the bottom materials with the materials in other parts. The linked control of the rotation speed and temperature enables the heat generated by the reaction to be transferred out in a timely manner in the high - temperature area, while further enhancing the mass transfer efficiency and promoting the progress of the reaction. Compared with a single stirring paddle or a stirring system with a fixed rotation speed, this dynamic stirring system can better adapt to the requirements of different stages of the reaction process for the stirring intensity, improving the overall performance of the reactor. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] The drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention and do not constitute a limitation to the present invention.

[0019] Figure 1 It is a schematic diagram of the overall structure of the reaction kettle.

[0020] Figure 2 It is a schematic diagram of the internal structure of the reaction kettle.

[0021] Figure 3 It is a schematic diagram of the structure of the multi-stage vortex nozzle.

[0022] In the figure: 1, stirring motor; 2, feeding port; 3, reaction kettle body; 4, first heating ring; 5, second heating ring; 6, third heating ring; 7, bracket; 8, vortex nozzle; 9, upper paddle; 10, lower paddle; 11, discharging port. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0023] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments.

[0024] In the description of the present invention, it should be understood that the orientation or positional relationship indicated by the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", etc. is based on the orientation or positional relationship shown in the drawings, and is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation to the present invention.

[0025] Referring to Figures 1 - 3 , a special reaction kettle for the cyclization modification of naphthyl aromatic hydrocarbons, comprising a reaction kettle body 3. A stirring motor 1 is arranged at the top of the reaction kettle body 3. A stirring rod is arranged at the output end of the stirring motor 1. The stirring rod extends into the reaction kettle body 3. Two groups of stirring paddles are arranged on the stirring rod. Multiple heating rings are arranged on the outer wall of the reaction kettle, and the multiple heating rings are independently arranged. The bottom of the reaction kettle body 3 is supported by a bracket 7, the bottom of the reaction kettle is lifted, and a discharging port 11 is arranged at the bottom.

[0026] In other preferred embodiments, a feeding port 2 is arranged at the top of the reaction kettle. A switch cover is arranged at the feeding port 2. A knob is arranged on the switch cover, and the knob is used to control the opening and closing of the switch cover.

[0027] In other preferred embodiments, a vortex nozzle 8 is provided at the top of the reaction kettle. The vortex nozzle 8 includes an upper inclined nozzle and a lower inclined nozzle. There are 4 - 6 groups of upper inclined nozzles, and conical spiral guide vanes are arranged inside the upper inclined nozzles; there are 4 - 6 groups of lower inclined nozzles; and conical spiral guide vanes are arranged inside the lower inclined nozzles.

[0028] Design a conical spiral nozzle (with 3 layers of spiral guide vanes inside). Combining with the Venturi effect, raw materials (such as naphthalene and alkylating reagents) form micron - level atomized droplets under high pressure, improving the dispersion efficiency (droplet size ≤ 50μm).

[0029] Install a multi - stage vortex nozzle on the feed pipeline of the reaction kettle to ensure that the raw materials can smoothly enter the nozzle under the action of a high - pressure pump. During actual operation, by adjusting the pressure of the high - pressure pump, the raw materials pass through the nozzle at an appropriate speed, forming micron - level atomized droplets and entering the reaction kettle. For example, for the reaction of naphthalene and alkylating reagents, according to the reaction kinetics and raw material characteristics, the pressure of the high - pressure pump can be set between 1 - 3 MPa to obtain the best dispersion effect.

[0030] In other preferred embodiments, the two sets of stirring paddles on the stirring rod are respectively an inclined - blade paddle and an anchor - type paddle. The anchor - type paddle is arranged below the inclined - blade paddle. There are 4 - 6 groups of inclined - blade paddles, and the blade inclination angle is 30 - 60°. The upper - layer inclined - blade paddles are used to enhance the axial flow and promote the dispersion of raw materials. The lower - layer anchor - type paddles are close to the kettle wall, enhancing the radial shear force, preventing material deposition, and at the same time enhancing the exchange of materials between the bottom material and other parts of the material.

[0031] The double - layer turbine stirring paddle is connected to the motor, and the motor is linked with the temperature control system through the control system. When the reaction enters the high - temperature zone, the temperature control system sends a signal to the motor control system, and the motor automatically increases the rotation speed to 800 - 1200 rpm. In the initial stage of the reaction or in the low - temperature zone, the motor maintains a lower rotation speed, such as 300 - 500 rpm. At the same time, according to the viscosity of the material in the reaction kettle and the reaction process, the angle and spacing of the stirring paddle can be appropriately adjusted to further optimize the stirring effect. The linked control of the rotation speed and temperature enables the heat generated by the reaction to be transferred out in time in the high - temperature zone, while further enhancing the mass transfer efficiency and promoting the progress of the reaction. Compared with a single - stirring - paddle or a stirring system with a fixed rotation speed, this dynamic stirring system can better adapt to the requirements of different stages of the reaction process for the stirring intensity, improving the overall performance of the reaction kettle.

[0032] In other preferred embodiments, there are three groups of heating rings, which are the first heating ring 4, the second heating ring 5, and the third heating ring 6 from top to bottom; they are arranged in the upper, middle, and lower layers of the reaction kettle body 3. Heat - conducting tubes are arranged inside the heating rings, and the heat - conducting tubes are connected to an external heat supply source. Temperature control components are arranged on the heat - conducting tubes.

[0033] Specifically, at least three temperature detectors are arranged inside the reactor body 3. The three temperature detectors are arranged on the stirring shaft and are respectively arranged corresponding to each layer of heating ring.

[0034] The annular heat conduction tube is connected to an independent temperature control device, and the temperature control device for each partition can be accurately regulated according to a preset temperature program. Before the reaction starts, according to the reaction process requirements, set the target temperatures of each axial region, such as 80 °C, 120 °C, 100 °C, etc. During the reaction process, the temperature of each region is monitored in real time through a temperature sensor, and the signal is fed back to the temperature control device. The temperature control device automatically adjusts the flow rate of the heating or cooling medium in the heat conduction tube according to the feedback signal to maintain the temperature of each region within the set accuracy range.

[0035] In other preferred embodiments, the material of the reactor body 3 is Hastelloy, and the wall thickness is 20 mm.

[0036] Example 2:

[0037] Reactor shape:

[0038] Dimensions: Vertical cylindrical, total height 1500 mm, diameter 800 mm, material is Hastelloy (HastelloyC-276), wall thickness 20 mm.

[0039] Nozzle position: A multi-stage vortex nozzle is installed at the top center, connected by a flange, and the outlet extends downward to the middle of the kettle.

[0040] Temperature control zone design:

[0041] Heat conduction tube layout: 3 groups of annular heat conduction rings (diameter 15 mm) are embedded in the inner wall of the kettle body, and the upper, middle and lower three zones are independently temperature controlled (temperature control accuracy ±0.5 °C).

[0042] Upper zone: 200 mm from the top, length 300 mm, calibrated temperature range 80 - 100 °C.

[0043] Middle zone: In the middle position, length 400 mm, calibrated temperature range 120 - 140 °C.

[0044] Lower zone: 200 mm from the bottom, length 300 mm, calibrated temperature range 90 - 110 °C.

[0045] Heat conduction medium interface: A heat conduction oil inlet (DN25) is provided at the bottom, and an outlet (DN25) is provided at the top.

[0046] Stirring system:

[0047] Double-layer turbine stirring paddle:

[0048] Upper paddle 9: Inclined blade turbine type, diameter 300 mm, blade inclination angle 45°, number of blades 4 - 6 pieces.

[0049] Lower paddle 10: Anchor paddle, with a diameter of 700 mm (close to the kettle wall) and a blade width of 80 mm.

[0050] Drive motor: Mounted on the top, with a power of 7.5 kW and a speed range of 200 - 1200 rpm (linked with temperature control).

[0051] Auxiliary interface:

[0052] Feeding port 2: At the upper part of the side wall, with a diameter of 80 mm, connected to a metering pump.

[0053] Pressure gauge: Mounted on the top, with a measuring range of 0 - 5 MPa.

[0054] Multi-stage vortex nozzle

[0055] Total length: 200 mm, designed with three-stage contraction:

[0056] Inlet section: With a diameter of 50 mm and a length of 60 mm, and a smooth inner wall.

[0057] Vortex section: With a diameter of 30 mm and a length of 100 mm, and equipped with 3 layers of spiral guide vanes (made of silicon carbide).

[0058] Guide vane parameters: The number of guide vanes per layer is 3, the spiral angle is 60°, the pitch is 20 mm, and the thickness of the guide vane is 2 mm.

[0059] Outlet section: With a diameter of 2 mm (the claim range is 0.5 - 2 mm), a length of 40 mm, and a tapered angle of 15°.

[0060] Connection method:

[0061] Fixed to the top of the reactor through a flange (the outer diameter of the flange is 120 mm, and the bolt holes are 8×M16).

[0062] The outer wall of the nozzle is coated with a heat insulation layer (ceramic fiber, with a thickness of 10 mm).

[0063] The above is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention, according to the technical solution and inventive concept of the present invention, makes equivalent substitutions or changes, and all should be covered within the protection scope of the present invention.

Claims

1. A special reactor for naphthyl arene cycloalkylation modification, characterized in that: It comprises a reactor body, a stirring motor is arranged on the top of the reactor body, a stirring rod is arranged at the output end of the stirring motor, the stirring rod extends into the reactor body, and two groups of stirring paddles are arranged on the stirring rod; the outer wall of the reactor is provided with multi-stage heating rings, and the multiple heating rings are arranged independently.

2. The special reactor for cycloalkylation modification of naphthyl arene according to claim 1, characterized in that: The top of the reactor is provided with a feed inlet, an opening and closing cover is provided at the feed inlet, and a knob is provided on the opening and closing cover, and the knob is used to control the opening and closing of the opening and closing cover.

3. The special reactor for cycloalkylation modification of naphthyl arene according to claim 1, characterized in that: A vortex nozzle is arranged on the top of the reaction kettle, and the vortex nozzle includes an upward inclined nozzle and a downward inclined nozzle. The upward inclined nozzle is arranged in 4-6 groups, and conical spiral guide vanes are arranged in the upward inclined nozzle; the downward inclined nozzle is arranged in 4-6 groups; and a conical spiral guide vane is arranged in the downward inclined nozzle.

4. The special reactor for cycloalkylation modification of naphthyl arene according to claim 1, characterized in that: The two groups of stirring paddles on the stirring rod are respectively a pitched-blade paddle and an anchor-type paddle. The anchor-type paddle is arranged below the pitched-blade paddle. There are 4 to 6 groups of pitched-blade paddles, and the blade inclination angle is 30 to 60 degrees.

5. The special reactor for cycloalkylation modification of naphthyl arene according to claim 1, characterized in that: The heating rings are provided in three groups, which are respectively arranged in the upper layer, the middle layer and the lower layer of the reactor body. A heat pipe is arranged in the heating ring, and the heat pipe is connected to an external heat source. A temperature control component is arranged on the heat pipe.

6. The special reactor for cycloalkylation modification of naphthyl arene according to claim 5, characterized in that: At least three groups of temperature detectors are arranged inside the reactor body. The three groups of temperature detectors are arranged on the stirring shaft and correspond to the heating rings of each layer.

7. The special reactor for cycloalkylation modification of naphthyl arene according to claim 1, characterized in that: The material of the reactor body is Hastelloy, and the wall thickness is 20 mm.