A fully automatic crude phenol production system and method for producing crude phenol

By adopting an adjustable stirring structure and cooling device in the crude phenol production system, the vortex and uniform heat problems during the stirring process are solved, efficient mixing and uniform heat are achieved, production efficiency and quality are improved, raw material loss and labor costs are reduced .

CN112691631BActive Publication Date: 2024-12-27MASTEEL ORSEA CHEM CO LTD
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Patent Information

Application Number
CN202011489314.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2020-12-16
Publication Date
2024-12-27
Estimated Expiration
2040-12-16

AI Technical Summary

Technical Problem

In the existing crude phenol production methods, vortex is prone to affect the reaction during the stirring process, poor uniform heat effect, resulting in excessive increase in air pressure and loss of raw materials, affecting production efficiency and quality.

Method used

Adopt a fully automatic crude phenol production system, including an adjustable stirring structure and cooling device, drive the stirrer and stirring structure to rotate through a stirring motor, and use the adjustment plate to change the stirring state, combine the water-cooled jacket and cooling water circulation system to achieve efficient mixing and uniformity. and the reaction conditions are monitored and adjusted through the control module.

Benefits of technology

High-efficiency mixing and uniform heat are achieved, raw material loss is avoided, production efficiency and quality control are improved, and labor costs are reduced.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses a fully automatic crude phenol production system and a method for producing crude phenol, and belongs to the field of crude phenol production. The system comprises a reactor, a sodium sulfate storage tank and a crude phenol storage tank connected to the reactor through a pipeline, a stirring motor is fixedly installed on the reactor, an output end of the stirring motor is fixedly connected to a stirrer arranged inside the reactor, a stirring structure whose position can be freely adjusted is provided on the stirrer, an adjustment plate for adjusting the state of the stirring structure is provided at a corresponding position on the inner wall of the reactor, a cooling device is provided on the outside of the reactor, and a sulfuric acid feeding port and a phenate feeding port are provided on the top of the reactor. The stirring structure is driven to rotate by the stirrer, and when the stirring structure touches the adjustment plate, the stirring state will be changed, so as to prevent a deeper vortex from appearing inside the reactor, ensure efficient mixing and reaction of sulfuric acid and phenate, and at the same time, efficiently heat evenly to avoid the loss of raw materials or generated crude phenol with the pressure discharge caused by uneven heating.
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Description

Technical Field

[0001] The present invention relates to the technical field, and in particular to a fully automatic crude phenol production system and a method for producing crude phenol. Background Art

[0002] Phenols are one of the main chemical products extracted from coal tar. Their composition and yield are related to conditions such as the composition and quality of the coal blend and the coking temperature. The higher the coking temperature, the lower the phenol yield and the less low-grade phenols. The phenol content in high-temperature tar fluctuates greatly, generally 2-4% of the tar, of which 60% is low-grade phenols.

[0003] At present, the production methods of crude phenol are mainly based on sulfuric acid method and carbon dioxide method. The production is carried out according to the principle of strong acid replacing weak acid, and separation is achieved by using solubility difference. The crude phenol obtained by separation is mainly phenol, cresol, xylenol, and higher phenol. Low-grade phenol, as an important chemical raw material, has been generally separated and extracted. However, there are related technical problems in the prior art: for example, stirring is required for mixing reaction and uniform heating effect when sulfuric acid is added. The stirring process is relatively simple, and vortexes will appear in the process to affect the reaction of sulfuric acid and phenol salt, and the poor uniform heating effect will cause the internal air pressure to rise too quickly. Some raw materials will be lost through the pipeline during pressure relief, which will inevitably affect production efficiency and production quality. Summary of the invention

[0004] The purpose of the present invention is to solve the deficiencies in the prior art. Therefore, a fully automatic crude phenol production system and a method for producing crude phenol are proposed. The system can efficiently heat and fully mix the crude phenol by adapting the stirring structure and the adjusting plate. The system is simple and easy to operate, and the cost and quality are controllable.

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

[0006] A fully automatic crude phenol production system comprises a reactor, a sodium sulfate storage tank and a crude phenol storage tank connected to the reactor through a pipeline, a stirring motor is fixedly installed on the reactor, an output end of the stirring motor is fixedly connected to a stirrer arranged inside the reactor, the stirrer is provided with a stirring structure whose position can be freely adjusted, an adjustment plate for adjusting the state of the stirring structure is arranged at a corresponding position on the inner wall of the reactor, a cooling device is arranged on the outer side of the reactor, and a sulfuric acid feeding port and a phenate feeding port are arranged on the top of the reactor.

[0007] According to a further preferred embodiment, the stirring structure includes a guide sleeve, a stirring main blade 1, a guide member, a stirring main blade 2 and a stirring auxiliary blade. The guide sleeve is integrally connected to the agitator and is arranged perpendicular to the axial direction of the agitator. The stirring main blade 1 is slidably arranged inside the guide sleeve and is located in the same horizontal plane as the adjustment plate. Both ends of the stirring main blade 1 are respectively rotatably connected to a pair of stirring auxiliary blades. Two stirring main blades 2 are symmetrically arranged and are respectively arranged on both sides of the stirring main blade 1. Both ends of the stirring main blade 2 are respectively rotatably connected to the corresponding stirring auxiliary blades. Two guide members are provided and are fixedly installed on the agitator along the axial direction of the agitator. The two stirring main blades 2 are respectively slidably matched with the corresponding guide members.

[0008] In a further preferred embodiment, the two main stirring blades are arranged in opposite directions to push the liquid to flow.

[0009] In a further preferred solution, the adjustment plate has an arc-shaped structure, and the distance between the adjustment plate and the center of the agitator gradually decreases along the rotation direction of the agitator.

[0010] In a further preferred embodiment, the cooling device comprises a water cooling jacket and a cooling water circulation system, the water cooling jacket is arranged on the outside of the reactor and connected to the cooling water circulation system through a pipeline, and a heat dissipation baffle fixedly arranged on the outer wall of the reactor is arranged on the inner side of the water cooling jacket.

[0011] In a further preferred embodiment, the heat dissipation baffle is arranged in a spiral structure, and the pitch of the spiral structure gradually decreases from top to bottom.

[0012] A further preferred solution also includes a control module, which includes a test unit and a control unit, wherein the test unit includes test points A, B, C and D, wherein the test point A is used to detect the temperature value inside the water-cooling jacket; the test point B is used to detect the temperature value, pH value and liquid level value inside the reactor; the test point C is used to detect the pH value of the feed port of the sodium sulfate storage tank; the test point D is used to detect the density value of the feed port of the sodium sulfate storage tank and the crude phenol storage tank, and the control unit is electrically connected to the test points A, B, C and D for controlling each speed regulating valve.

[0013] The present invention also discloses a method for producing crude phenol in a fully automatic crude phenol production system, comprising the following steps:

[0014] Step 1: input raw material phenol salt parameters and planned crude phenol production data into the setting control module, and the control module automatically controls the speed regulating valve at the phenol salt feeding port to open until a certain amount of phenol salt raw material is added into the reactor and then closed;

[0015] Step 2: The control module controls the stirring motor to start and stirs the phenolate through the agitator and the stirring structure. When the stirring main blade 1 contacts the adjustment plate, the stirring structure gradually changes its stirring state along the rotation direction of the agitator, drives the stirring main blade 2 to move in the opposite direction and realizes convection. At the same time, the speed regulating valve at the sulfuric acid feeding port is opened and the reactor is roughly fed at a flow rate of 10L / min until the temperature rise gradient measured at the test point B meets the design requirements. Subsequently, the sulfuric acid feeding port is finely fed through the speed regulating valve there until the pH value of the mixed solution inside the reactor meets the design requirements. During the process, the test point A detects the temperature inside the water-cooling jacket 13 and feeds it back to the control module. The control module controls the speed regulating valve to indirectly control the cooling effect of the water-cooling jacket 13;

[0016] Step 3: Stir for 0.5h and then let stand for 1h. After the pH value of the reaction product measured by test point C meets the design requirements, the reactor starts to discharge. If the density value measured by test point D meets the density requirements of sodium sulfate, the feed inlet regulating valve of the sodium sulfate storage tank is opened and the feed inlet regulating valve of the crude phenol storage tank is closed; if the density value measured by test point D meets the density requirements of crude phenol, the feed inlet regulating valve of the crude phenol storage tank is opened and the feed inlet regulating valve of the sodium sulfate storage tank is closed;

[0017] Step 4: The production process ends when the reactor is emptied, that is, the density value measured at test point D is zero.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] The present invention is provided with a state-variable stirring structure and an adjustment plate corresponding to the position of the stirring structure. The stirring structure is driven to rotate by a stirrer. When the stirring structure touches the adjustment plate, the stirring state is changed to prevent the appearance of a deep vortex inside the reactor, thereby ensuring efficient mixing and reaction of sulfuric acid and phenol salt. At the same time, it can also efficiently heat evenly to avoid the loss of raw materials or generated crude phenol with the pressure relief discharge due to uneven heating.

[0020] The stirring structure in the present invention adopts a guide sleeve, a stirring main blade 1, a guide member, a stirring main blade 2 and a stirring auxiliary blade. The two ends of the stirring main blade 1 are rotated to a suitable position (when contacting the adjustment plate), and the stirring main blade 1 will change its position. At the same time, the stirring auxiliary blade drives the two stirring main blades 2 to realize periodic reciprocating motion up and down along the corresponding guide member, thereby controlling the internal stirring uniformity and achieving efficient stirring and uniform heating effects.

[0021] In the present invention, the flow directions of the liquid pushed by the second stirring main blade are arranged relatively to form an upper and lower circulating vortex structure and produce a collision in the middle, thereby realizing the function of sufficient mixing and stirring. While stirring, the sulfuric acid on the top can also flow downward for uniform heating and sufficient mixing reaction, and the liquid at the bottom will also flow upward with the liquid. At the same time, the internal adjustment plate and the first stirring main blade and the stirring auxiliary blade destroy the vortex, thereby further realizing efficient uniform heating and material mixing and reaction.

[0022] The cooling device in the present invention includes a water-cooling jacket and a cooling water circulation system, as well as a heat dissipation baffle (special design structure) arranged on the outer wall of the reactor and located inside the jacket, which effectively cools the reactor and greatly reduces the loss of raw materials and materials during pressure relief.

[0023] The present invention tests multiple test points through a control module, thereby ensuring fully automated production of crude phenol with precise control, greatly reducing labor costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0025] Figure 2 It is a schematic diagram of the internal structure of the reactor of the present invention;

[0026] Figure 3 It is a top view of the internal structure of the reactor of the present invention;

[0027] Figure 4 It is a schematic diagram of the overall structure of the heat dissipation baffle inside the water-cooling jacket of the present invention.

[0028] In the figure: 1. Reactor; 2. Sodium sulfate storage tank; 3. Crude phenol storage tank; 4. Heat dissipation baffle; 5. Stirring motor; 6. Adjustment plate; 7. Sulfuric acid feeding port; 8. Phenol salt feeding port; 9. Guide sleeve; 10. Stirring main blade 1; 11. Stirring auxiliary blade; 12. Agitator; 13. Water cooling jacket; 14. Cooling water circulation system; 15. Stirring main blade 2; 16. Guide piece. DETAILED DESCRIPTION

[0029] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0030] In the description of the present invention, it is necessary to understand that the terms "upper", "lower", "front", "back", "left", "right", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship are based on the orientation or position relationship shown in the drawings, and are 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 cannot be understood as a limitation on the present invention.

[0031] Example 1

[0032] like Figures 1 to 4 As shown, a fully automatic crude phenol production system comprises a reactor 1, a sodium sulfate storage tank 2 and a crude phenol storage tank 3 connected to the reactor 1 through a pipeline, a stirring motor 5 is fixedly installed on the reactor 1, an output end of the stirring motor 5 is fixedly connected to a stirrer 12 arranged inside the reactor 1, a stirring structure whose position can be freely adjusted is arranged on the stirrer 12, an adjustment plate 6 for adjusting the state of the stirring structure is arranged at a corresponding position on the inner wall of the reactor 1, a cooling device is arranged on the outside of the reactor 1, and a sulfuric acid feeding port 7 and a phenolate feeding port 8 are arranged on the top of the reactor 1. The stirring motor 5 is used to drive the stirring structure to rotate, and when the stirring structure rotates to the position of the adjustment plate 6, the state will be changed under the action of the adjustment plate 6, and then the periodic reciprocating irregular motion will be realized, which greatly improves its mixing efficiency and facilitates the realization of a full reflection effect, and can also effectively evenly heat, so that the cooling device can be convenient for cooling the inside, reduce the excessive increase in pressure when sulfuric acid is added, and effectively reduce the loss of materials during pressure discharge.

[0033] In the present embodiment, a further preferred scheme is that the stirring structure includes a guide sleeve 9, a stirring main blade 10, a guide member 16, a stirring main blade 2 15 and a stirring auxiliary blade 11. The guide sleeve 9 is integrally connected to the agitator 12 and is arranged perpendicular to the axial direction of the agitator 12. The stirring main blade 10 is slidably arranged inside the guide sleeve 9 and is located in the same horizontal plane as the adjustment plate 6. A pair of stirring auxiliary blades 11 are rotatably connected to the two ends of the stirring main blade 10 respectively. Two stirring main blades 15 are symmetrically arranged and are respectively arranged on both sides of the stirring main blade 10. The two ends of the stirring main blade 2 15 are respectively rotatably connected to the corresponding stirring auxiliary blades 11. The guide members 16 are provided with two and are fixedly installed on the agitator 12 along the axial direction of the agitator 12. The two stirring main blades 15 are respectively slidably matched with the corresponding guide members 16. The guide member 16 is columnar and has a cross-shaped cross-section. When the end of the stirring main blade 10 contacts the adjustment plate 6, it will move to the other end. At the same time, the stirring auxiliary blade 11 will make the stirring main blade 15 move in the opposite direction to the guide member 16 (at the same time, toward the side close to the stirring main blade 10 or away from the stirring main blade 10). This can increase the stirring contact area and eliminate the disadvantages of traditional stirring that the vortex is too deep and cannot be fully mixed and reacted, which greatly promotes the production efficiency of crude phenol and ensures the technical effect of its production quality.

[0034] In a further preferred embodiment of the present invention, the two stirring main blades 15 are arranged opposite to each other in the direction of pushing the liquid. This special design can make the vortex generated by the upper and lower stirring main blades 15 convect at the stirring main blade 10 to achieve full mixing and reaction.

[0035] In this embodiment, the adjustment plate 6 has an arc structure, and the distance between the adjustment plate 6 and the center of the stirrer 12 gradually decreases along the rotation direction of the stirrer 12. This makes the movement of the stirring main blade 15 change irregularly, thereby changing the directional movement of the liquid inside the reactor 1, so that the liquid is heated evenly and mixed and reacted fully.

[0036] In a further preferred solution of this embodiment, the cooling device includes a water cooling jacket 13 and a cooling water circulation system 14, the water cooling jacket 13 is arranged outside the reactor 1 and connected to the cooling water circulation system 14 through a pipeline, and a heat dissipation baffle 15 fixedly arranged on the outer wall of the reactor 1 is arranged inside the water cooling jacket 13. The cooling water circulation system is used to pass cooling water into the water cooling jacket 13, and the heat inside the reactor 1 is removed through the cooling water and the heat dissipation baffle 15 for heat exchange.

[0037] In the embodiment, the heat dissipation baffle 15 is arranged in a spiral structure, and the pitch of the spiral structure gradually decreases from top to bottom. With the special design of the spiral pitch, since sulfuric acid is generally added from top to bottom, the heat will be generated at the top first, and it is necessary to take away the heat in time, otherwise acid mist will be generated and will take away the material when the pressure is discharged, which will waste costs and be detrimental to production. At this time, a large amount of cooling water is concentrated on the top to take away the internal temperature, thereby effectively controlling the internal pressure and ensuring production costs and quality.

[0038] A further preferred solution in this embodiment also includes a control module, which includes a test unit and a control unit. The test unit includes test points A, B, C and D. The test point A is used to detect the temperature value inside the water-cooling jacket 13, that is, to control the pressure and cooling conditions inside it; the test point B is used to detect the temperature value, pH value and liquid level value inside the reactor 1, and the reaction conditions inside the reactor 1 are evaluated through three test objects; the test point C is used to detect the pH value of the feed port of the sodium sulfate storage tank 2, and this point determines whether it is the final reaction of the theoretical design; the test point D is used to detect the density value of the feed port of the sodium sulfate storage tank 2 and the crude phenol storage tank 3, and this point test is to control the flow direction of the product, and the control unit is electrically connected to the test points A, B, C and D for controlling each speed regulating valve.

[0039] Embodiment 2:

[0040] A method for producing crude phenol in a fully automatic crude phenol production system comprises the following steps:

[0041] Step 1: input raw material phenol salt parameters and planned crude phenol production data into the setting control module, and the control module automatically controls the speed regulating valve at the phenol salt feeding port 8 to open until a certain amount of phenol salt raw material is added into the reactor 1 and then closed;

[0042] Step 2: The control module controls the stirring motor 5 to start and stir the phenolate through the agitator 12 and the stirring structure. When the stirring main blade 10 contacts the adjustment plate 6, the stirring structure gradually changes its stirring state along the rotation direction of the agitator 12, drives the stirring main blade 2 15 to move in the opposite direction and realizes convection. At the same time, the speed regulating valve at the sulfuric acid feeding port 7 is opened and the reaction kettle 1 is roughly fed at a flow rate of 10L / min until the temperature rise gradient measured at the test point B meets the design requirements. Subsequently, the sulfuric acid feeding port 7 is finely fed through the speed regulating valve therein until the pH value of the mixed solution inside the reaction kettle 1 meets the design requirements. During the process, the test point A detects the temperature inside the water-cooling jacket 13 and feeds it back to the control module. The control module controls the speed regulating valve to indirectly control the cooling effect of the water-cooling jacket 13;

[0043] Step 3: Stir for 0.5h and then let stand for 1h. After the pH value of the reaction product measured by test point C meets the design requirements, the reactor 1 starts to discharge. If the density value measured by test point D meets the density requirement of sodium sulfate, the feed inlet regulating valve of sodium sulfate storage tank 2 is opened and the feed inlet regulating valve of crude phenol storage tank 3 is closed; if the density value measured by test point D meets the density requirement of crude phenol, the feed inlet regulating valve of crude phenol storage tank 3 is opened and the feed inlet regulating valve of sodium sulfate storage tank 2 is closed;

[0044] Step 4: The production process ends when the interior of the reactor 1 is emptied, that is, the density value measured at the test point D is zero.

[0045] The above is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. The replacement may be a replacement of a part of the structure, device, method step, or a complete technical solution. Any equivalent replacement or change according to the technical solution and the inventive concept of the present invention shall be covered within the protection scope of the present invention.

Claims

1. A fully automatic crude phenol production system, comprising a reactor (1), a sodium sulfate storage tank (2) and a crude phenol storage tank (3) connected to the reactor (1) through a pipeline, characterized in that: The reactor (1) is fixedly provided with a stirring motor (5), the output end of the stirring motor (5) is fixedly connected with a stirrer (12) arranged inside the reactor (1), the stirrer (12) is provided with a stirring structure whose position can be freely adjusted, an adjustment plate (6) for adjusting the state of the stirring structure is provided at a corresponding position on the inner wall of the reactor (1), a cooling device is provided on the outer side of the reactor (1), and a sulfuric acid feeding port (7) and a phenate feeding port (8) are provided on the top of the reactor (1); The stirring structure comprises a guide sleeve (9), a stirring main blade (10), a guide member (16), a stirring main blade (2) and a stirring auxiliary blade (11); the guide sleeve (9) is integrally connected to the stirrer (12) and is arranged perpendicular to the axial direction of the stirrer (12); the stirring main blade (10) is slidably arranged inside the guide sleeve (9) and is located in the same horizontal plane as the adjustment plate (6); a pair of stirring auxiliary blades (11) are rotatably connected at both ends of the stirring main blade (10); two stirring main blades (2) are symmetrically arranged and are respectively arranged on both sides of the stirring main blade (10); the two ends of the stirring main blade (2) are respectively rotatably connected to the corresponding stirring auxiliary blades (11); two guide members (16) are provided and are fixedly installed on the stirrer (12) along the axial direction of the stirrer (12); the two stirring main blades (2) are respectively slidably matched with the corresponding guide members (16).

2. A fully automatic crude phenol production system according to claim 1, characterized in that: The two stirring main blades 2 (15) push the liquid to flow in opposite directions.

3. A fully automatic crude phenol production system according to claim 2, characterized in that: The adjustment plate (6) is an arc-shaped structure, and the distance between the adjustment plate (6) and the center of the stirrer (12) gradually decreases along the rotation direction of the stirrer (12).

4. A fully automatic crude phenol production system according to claim 3, characterized in that: The cooling device comprises a water cooling jacket (13) and a cooling water circulation system (14); the water cooling jacket (13) is arranged on the outside of the reaction kettle (1) and connected to the cooling water circulation system (14) through a pipeline; the inside of the water cooling jacket (13) is provided with a heat dissipation baffle (4) fixedly arranged on the outer wall of the reaction kettle (1).

5. A fully automatic crude phenol production system according to claim 4, characterized in that: The heat dissipation baffle (4) is arranged in a spiral structure, and the pitch of the spiral structure gradually decreases from top to bottom.

6. A fully automatic crude phenol production system according to claim 5, characterized in that: The invention also comprises a control module, wherein the control module comprises a test unit and a control unit, wherein the test unit comprises test points A, B, C and D, wherein the test point A is used to detect the temperature value inside the water-cooling jacket (13); the test point B is used to detect the temperature value, pH value and liquid level value inside the reactor (1); the test point C is used to detect the pH value at the feed port of the sodium sulfate storage tank (2); the test point D is used to detect the density value at the feed ports of the sodium sulfate storage tank (2) and the crude phenol storage tank (3), and the control unit is electrically connected to the test points A, B, C and D for controlling each speed regulating valve.

7. The method for producing crude phenol according to claim 6, characterized in that: The following steps are involved: Step 1: inputting raw material phenol salt parameters and planned crude phenol production data into the setting control module, the control module automatically controls the speed regulating valve at the phenol salt feeding port (8) to open until a certain amount of phenol salt raw material is added into the reactor (1) and then closes; Step 2: The control module controls the stirring motor (5) to start and stir the phenol salt through the stirrer (12) and the stirring structure. When the stirring main blade 1 (10) contacts the adjustment plate (6), the stirring structure gradually changes its stirring state along the rotation direction of the stirrer (12). The stirring auxiliary blade (11) drives the stirring main blade 2 (15) to approach each other and realize liquid convection. At the same time, the speed regulating valve at the sulfuric acid feeding port (7) is opened and the reaction kettle (1) is roughly fed at a flow rate of 10L / min until the temperature rise gradient measured at the test point B meets the design requirements. Then, the sulfuric acid feeding port (7) is finely fed through the speed regulating valve there, until the pH value of the mixed solution in the reaction kettle (1) meets the design requirements. During the process, the test point A detects the temperature inside the water cooling jacket (13) and feeds it back to the control module. The control module controls the speed regulating valve to indirectly control the cooling effect of the water cooling jacket (13); Step 3: After stirring for 0.5 h, let it stand for 1 h. After the pH value of the reaction product measured at test point C meets the design requirements, the reactor (1) starts to discharge. If the density value measured at test point D meets the density requirements of sodium sulfate, the feed inlet regulating valve of the sodium sulfate storage tank (2) is opened and the feed inlet regulating valve of the crude phenol storage tank (3) is closed; if the density value measured at test point D meets the density requirements of crude phenol, the feed inlet regulating valve of the crude phenol storage tank (3) is opened and the feed inlet regulating valve of the sodium sulfate storage tank (2) is closed; Step 4: The production process ends when the interior of the reactor (1) is emptied, that is, the density value measured at the test point D is zero.