Production device and process of terpene-phenol resin

Abstract

The invention relates to the technical field of terpene-phenolic resin production, in particular to a production device and process of terpene-phenolic resin. The production device is characterized by comprising a phenol storage tank, a reaction kettle, a first receiver, a second receiver and an oil-water separator, by designing structures of a first receiver, a second receiver, an oil-water separator and the like, designing a specific pipeline connecting structure, combining with the position design of each electric control valve, matching with a specific production method and through different temperature stages in the reaction kettle, the corresponding electric control valves are controlled to be opened or closed respectively, and the phenol and heavy oil are separated from each other by utilizing the difference of boiling points of phenol and heavy oil. The first receiver is used for collecting phenol and heavy oil in two stages respectively, so that the evaporated phenol and heavy oil in the reaction kettle are fully separated and recycled.

Description

Technical Field

[0001] This invention relates to the field of terpene phenol resin production technology, and more particularly to the production apparatus and process for terpene phenol resin. Background Technology

[0002] Chinese patent CN203807374U discloses a circulating terpene phenol resin production device that achieves the separation and recovery of phenol and heavy oil in the reactor. However, in the above patent solution, the heavy oil is directly introduced into the waste oil collection tank through a separate pipeline. This makes it impossible to fully utilize the cooling mechanism of the second pipeline when collecting waste oil. Furthermore, the simultaneous collection of heavy oil and phenol can easily lead to some phenol condensing and flowing into the waste oil collection tank. The separation and recovery process can easily lead to the mixing of phenol and heavy oil, making it difficult to directly recover the phenol as a reaction raw material. Summary of the Invention

[0003] The technical problem to be solved by this invention is to improve the production equipment and process of terpene phenol resin so that the phenol and heavy oil evaporated in the reaction vessel can be fully separated and recovered.

[0004] To solve the above-mentioned technical problems, the technical solution adopted by the present invention is as follows:

[0005] The production equipment for terpene phenol resin includes a phenol storage tank, a reaction vessel, a first acceptor, a second acceptor, and an oil-water separator;

[0006] The phenol storage tank is connected to the reaction vessel via a feed pipe;

[0007] The reactor and the first receiver are connected by a first pipe, which includes an inclined rising section and an inclined falling section arranged sequentially from the reactor toward the first receiver. The inclined falling section is equipped with a cooling device.

[0008] The upper part of the first receiver is connected to the upper part of the second receiver through the second pipe, and the second pipe is connected to the first solenoid valve;

[0009] It also includes a third pipeline, the main branch of which is connected at the lower part of the rising section of the first pipeline, and at the upper part of the oil-water separator. The main branch of the third pipeline is connected to a first branch and a second branch. The first branch is connected to the lower part of the first receiver, and the second branch is connected to the upper part of the second receiver. A second electrically controlled valve is provided at the beginning of the main branch. A third electrically controlled valve is provided at the front of the branching part of the main branch relative to the first branch. A fourth electrically controlled valve is provided at the position of the second branch near the main branch. A fifth electrically controlled valve is provided at the position of the main branch relative to the branching part of the second branch. The second receiver is connected to the phenol storage tank through a fourth pipeline, which is connected to a material pump and a sixth electrically controlled valve.

[0010] The upper part of the first receiver is connected to a vacuum tube, which is connected to a seventh electrically controlled valve.

[0011] Furthermore, in the above-mentioned structure of the terpene phenol resin production apparatus, the height of the first acceptor is higher than the height of the reaction vessel.

[0012] Furthermore, in the above-mentioned terpene phenol resin production apparatus structure, the height of the second receiver is lower than the height of the reaction vessel.

[0013] Furthermore, in the above-mentioned terpene phenol resin production device structure, the height of the oil-water separator is consistent with the height of the second receiver.

[0014] Furthermore, in the above-mentioned terpene phenol resin production apparatus structure, the height of the phenol storage tank is higher than the height of the reaction vessel.

[0015] Furthermore, the above-mentioned terpene phenol resin production device structure also includes a circulation balance pipe, the beginning of which is connected to the upper part of the first receiver and the end of which is connected to the inclined descending section of the first pipeline.

[0016] This invention also relates to a method for producing terpene phenol resins. Based on the above-described apparatus for producing terpene phenol resins, the method includes the following steps:

[0017] S1: Inputting the reaction raw materials into the reaction vessel, including metering the phenol from the phenol storage tank into the reaction vessel;

[0018] S2: Control the continuous heating of the reactor. When the temperature inside the reactor is in the range of 150-250℃, the first, second, third, fourth, fifth, and sixth electric control valves are closed, and the seventh electric control valve is opened, so that the first receiver is in a negative pressure vacuum state. The first receiver is connected to the reactor, forming a suction effect, so that the gaseous phenol in the reactor is cooled into liquid through the first pipe and enters the first receiver.

[0019] S3: When the temperature inside the reactor reaches 250℃, maintain the temperature at 250℃, control the first solenoid valve to open, so that the second receiver and the first receiver are both in a negative pressure state; after a preset time, control the fourth solenoid valve to open, so that the phenol collected in the first receiver is discharged to the second receiver by gravity; after a preset time, control the fourth solenoid valve to close.

[0020] S4: The reactor continues to heat up to 270°C and maintains the temperature at 270°C. During this period, the second and third electric control valves are opened, so that part of the high-boiling-point heavy oil vapor in the reactor is condensed through the first pipe and enters the first receiver from the top, while the other part enters the first receiver from the bottom through the third pipe.

[0021] S5: The reactor discharges and samples every 2 hours to test the degree of reaction of the product. Once the product reaches the predetermined degree of reaction, the reactor stops heating and discharges the product. At the same time, the fifth electric control valve is opened to allow the high-boiling-point heavy oil in the first receiver to enter the oil-water separator for processing through the third pipeline.

[0022] Furthermore, in the above-mentioned method for producing terpene phenol resin, step S4 further includes: controlling the opening of the sixth electrically controlled valve and controlling the opening of the material pump, so that the phenol in the second receiver is pumped into the phenol storage tank.

[0023] The beneficial effects of this invention are as follows: by designing structures such as the first receiver, the second receiver, and the oil-water separator, and by designing specific pipeline connection structures combined with the position design of each electrically controlled valve, and in conjunction with specific production methods, the corresponding electrically controlled valves are opened or closed at different temperature stages in the reactor. By utilizing the difference in boiling points between phenol and heavy oil, segmented collection is achieved. The first receiver serves two functions in the two stages: collecting phenol and collecting heavy oil, respectively, so that the evaporated phenol and heavy oil in the reactor are fully separated and recovered. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of a production apparatus for terpene phenol resin according to a specific embodiment of the present invention;

[0025] Label Explanation:

[0026] 1. Phenol storage tank;

[0027] 2. Reactor;

[0028] 3. First receptor;

[0029] 4. Second receiver;

[0030] 5. Oil-water separator;

[0031] 6. First pipe; 61. Inclined rising section; 62. Inclined descending section; 621. Cooling device;

[0032] 7. Second pipeline; 71. First electrically controlled valve;

[0033] 8. Third pipeline; 81. Main pipeline; 82. First branch pipeline; 83. Second branch pipeline; 84. Second electrically controlled valve; 85. Third electrically controlled valve; 86. Fourth electrically controlled valve; 87. Fifth electrically controlled valve;

[0034] 9. Fourth pipeline; 91. Material pump; 92. Sixth electrically controlled valve;

[0035] 10. Vacuum tube; 101. Seventh solenoid valve;

[0036] 11. Circulation balance pipe;

[0037] 12. Rosin storage tank. Detailed Implementation

[0038] To explain in detail the technical content, objectives, and effects of the present invention, the following description is provided in conjunction with the embodiments and accompanying drawings.

[0039] Please refer to Figure 1 The present invention relates to a production apparatus for terpene phenol resin, comprising a phenol storage tank 1, a reaction vessel 2, a first receiver 3, a second receiver 4, and an oil-water separator 5;

[0040] The phenol storage tank 1 is connected to the reaction vessel 2 via a feed pipe;

[0041] The reactor 2 and the first receiver 3 are connected by a first pipe 6. The first pipe 6 includes an inclined rising section 61 and an inclined falling section 62 arranged sequentially from the reactor 2 to the first receiver 3. The inclined falling section 62 is provided with a cooling device 621.

[0042] The upper part of the first receiver 3 is connected to the upper part of the second receiver 4 through the second pipe 7, and the second pipe 7 is connected to the first solenoid valve 71.

[0043] It also includes a third pipe 8, the main channel 81 of which is connected at the beginning to the lower part of the rising section of the first pipe 6, and at the end to the upper part of the oil-water separator 5. The main channel 81 of the third pipe 8 is connected to a first branch channel 82 and a second branch channel 83. The first branch channel 82 is connected to the lower part of the first receiver 3, and the second branch channel 83 is connected to the upper part of the second receiver 4. A second electrically controlled valve 84 is provided at the beginning of the main channel 81. A third electrically controlled valve 85 is provided at the front of the branching part of the main channel 81 relative to the first branch channel 82. A fourth electrically controlled valve 86 is provided at the position of the second branch channel 83 near the main channel 81. A fifth electrically controlled valve 87 is provided at the rear of the branching part of the main channel 81 relative to the second branch channel. The second receiver 4 is connected to the phenol storage tank 1 through a fourth pipe 9, which is connected to a material pump 91 and a sixth electrically controlled valve 92.

[0044] The upper part of the first receiver 3 is connected to a vacuum tube 10, and the vacuum tube 10 is connected to a seventh electrically controlled valve 101.

[0045] The above embodiments also include a rosin storage tank 12 and other raw material storage tanks, which are connected to the reaction vessel 2 through corresponding pipes to realize automatic feeding of the reaction. The cooling device 621 mentioned above can be a condensing sleeve sleeved to the inclined descending section 62 of the first pipe 6. Cooling water of the corresponding temperature is introduced into the condensing sleeve, and the gaseous phenol passing through is condensed into liquid through heat transfer.

[0046] Preferably, the height of the first receiver 3 is higher than the height of the reactor 2.

[0047] Preferably, in the above-mentioned structure of the terpene phenol resin production apparatus, the height of the second receiver 4 is lower than the height of the reaction vessel 2.

[0048] Preferably, the height of the oil-water separator 5 is the same as the height of the second receiver 4.

[0049] Preferably, the height of the phenol storage tank 1 is higher than the height of the reaction vessel 2.

[0050] Preferably, it also includes a circulation balancing pipe 11, the beginning of which is connected to the upper part of the first receiver 3, and the end is connected to the inclined descending section 62 of the first pipe 6.

[0051] This invention also relates to a method for producing terpene phenol resins. Based on the above-described apparatus for producing terpene phenol resins, the method includes the following steps:

[0052] S1: Inputting the reaction raw materials into the reaction vessel 2, including metering the phenol in the phenol storage tank 1 into the reaction vessel 2;

[0053] Specifically, rosin is added to reactor 2, nitrogen is introduced for purging, and the temperature is raised to 150°C to melt it. Then, phenol is introduced into reactor 2, the temperature is lowered to 100°C, M is added, the temperature is raised to 150°C, and after stabilizing for 4 hours, samples are taken to test the viscosity. When the viscosity is greater than 360s (25°C), that is, the viscosity is qualified, C and soft water are mixed and added to the reactor, and stirred for 30 minutes.

[0054] S2: Control the continuous heating of reactor 2. When the temperature inside reactor 2 is in the range of 150-250℃, the first solenoid valve 71 closes, the second solenoid valve 84 closes, the third solenoid valve 85 closes, the fourth solenoid valve 86 closes, the fifth solenoid valve 87 closes, the sixth solenoid valve 92 closes, and the seventh solenoid valve 101 opens, so that the first receiver 3 is in a negative pressure vacuum state. The first receiver 3 is connected to reactor 2, forming a suction effect, so that the gaseous phenol in reactor 2 is cooled into liquid state through the first pipe 6 and enters the first receiver 3.

[0055] Specifically, the process involves adjusting the vacuum level to 0.085-0.09 MPa, simultaneously evacuating the vacuum and raising the temperature to 200°C over 3-5 hours, then releasing the vacuum and adding T; then continuing to evacuate the vacuum and raise the temperature to 250°C over 3-4 hours, releasing the vacuum and adding A and B, while simultaneously taking samples to test the softening point, acid value, and color number.

[0056] S3: When the temperature inside the reactor 2 reaches 250℃, maintain the temperature at 250℃, control the first solenoid valve 71 to open, so that the second receiver 4 and the first receiver 3 are both in a negative pressure state; after a preset time, control the fourth solenoid valve 86 to open, so that the phenol collected in the first receiver 3 is discharged to the second receiver 4 by gravity; after a preset time, control the fourth solenoid valve 86 to close.

[0057] Specifically, when the temperature is raised to 250℃, A and B are added under vacuum, and samples are taken to test the softening point, acid value and color number.

[0058] S4: The reactor 2 continues to be heated until it reaches 270°C, and then maintains the temperature at 270°C. During this period, the second solenoid valve 84 and the third solenoid valve 85 are opened, so that part of the high-boiling-point heavy oil vapor in the reactor 2 is condensed through the first pipe 6 and enters the first receiver 3 from the top, while the other part enters the first receiver 3 from the bottom through the third pipe 8.

[0059] Specifically, the reactor is continuously evacuated and heated, reaching 270℃ in 2-3 hours.

[0060] S5: Reactor 2 discharges and samples every 2 hours to test the degree of reaction of the product. Once the product reaches the predetermined degree of reaction, reactor 2 stops heating and discharges the product. At the same time, it controls the fifth electric control valve 87 to open, so that the high-boiling-point heavy oil in the first receiver 3 enters the oil-water separator 5 through the third pipe 8 for processing.

[0061] Specifically, when the temperature of the reactor reaches 270℃, it is kept at that temperature, and sampling is started to test the softening point and acid value until they are qualified.

[0062] The following steps are also included:

[0063] S6: After the softening point and acid value of the sample are qualified, cool down to 240℃, add D, stir for 15 minutes, then filter through a 150-mesh screen and sample to test the softening point, acid value, color number, and other indicators. (Softening point SP: 145-160; Acid value AV: 45-60; Color number: <7)

[0064] In the above embodiments, stage S2 is the period when phenol volatilizes. Through the action of vacuum tube 10, the first receiver 3 is made into a negative pressure state, thereby creating a suction effect on the reactor 2. The phenol volatilized products generated in the reactor 2 are introduced into the first receiver 3 through the first pipe 6. During this process, phenol is condensed into liquid under the action of cooling device 621 and falls into the first receiver 3 for collection.

[0065] In stage S3, the temperature of reactor 2 is controlled at 250℃. Below 250℃, heavy oil will not enter the first receiver 3 from the top through the first pipe 6. Even if a small amount of heavy oil volatiles condense and flow back to reactor 2 in the inclined rising section 61 of the first pipe 6, at the critical temperature of 250℃, the first solenoid valve 71 is opened to connect the second receiver 4 and the first receiver 3, both under negative pressure. After a preset time, the fourth solenoid valve 86 is opened to allow the phenol collected in the first receiver 3 to be discharged by gravity and flow to the second receiver 4. After a preset time, the fourth solenoid valve 86 is closed to allow the phenol liquid in the first receiver 3 to be fully introduced into the second receiver 4.

[0066] In stage S4, the reactor 2 continues to heat up to 270°C. This stage is the heavy oil collection stage because phenol has been completely recovered when the temperature is below 250°C. In the heavy oil recovery stage, part of the heavy oil enters the first receiver 3 from the top through the first pipe 6 and the other part enters the first receiver 3 from the bottom through the third pipe 8. That is, the two inclined sections of the first pipe 6 are used to condense and recover the heavy oil, so that the heavy oil is fully and efficiently recovered.

[0067] In stage S5, reactor 2 is maintained at 270℃. Periodic sampling and testing are conducted to check if the product in reactor 2 meets the required standards, thus determining the reaction endpoint. During this process, the heavy oil collection method from stage S4 is maintained. After the reaction is complete, reactor 2 stops heating and discharges the material. Simultaneously, the fifth electrically controlled valve 87 is opened, allowing the high-boiling-point heavy oil in the first receiver 3 to enter the oil-water separator 5 through the third pipe 8 for processing. This achieves efficient separate collection of heavy oil and phenol.

[0068] Preferably, S4 further includes: controlling the sixth electrically controlled valve 92 to open, controlling the material pump 91 to open, so that the phenol in the second receiver 4 is pumped into the phenol storage tank 1.

[0069] In the above embodiments, during the heavy oil recovery stage of S4, the phenol in the second receiver 4 can be pumped into the phenol storage tank 1 as a reaction raw material. This process will not interfere with the heavy oil recovery and further improves efficiency.

[0070] The above description is merely an embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent modifications made based on the content of the present invention specification and drawings, or direct or indirect applications in related technical fields, are similarly included within the patent protection scope of the present invention.

Claims

1. A production apparatus for terpene phenol resin, characterized in that, Includes phenol storage tank, reaction vessel, first receiver, second receiver and oil-water separator; The phenol storage tank is connected to the reaction vessel via a feed pipe; The reactor and the first receiver are connected by a first pipe, which includes an inclined rising section and an inclined falling section arranged sequentially from the reactor toward the first receiver. The inclined falling section is equipped with a cooling device. The upper part of the first receiver is connected to the upper part of the second receiver through the second pipe, and the second pipe is connected to the first solenoid valve; It also includes a third pipeline, the main branch of which is connected at the lower part of the rising section of the first pipeline, and at the upper part of the oil-water separator. The main branch of the third pipeline is connected to a first branch and a second branch. The first branch is connected to the lower part of the first receiver, and the second branch is connected to the upper part of the second receiver. A second electrically controlled valve is provided at the beginning of the main branch. A third electrically controlled valve is provided at the front of the branching part of the main branch relative to the first branch. A fourth electrically controlled valve is provided at the position of the second branch near the main branch. A fifth electrically controlled valve is provided at the position of the main branch relative to the branching part of the second branch. The second receiver is connected to the phenol storage tank through a fourth pipeline, which is connected to a material pump and a sixth electrically controlled valve. The upper part of the first receiver is connected to a vacuum tube, which is connected to a seventh electrically controlled valve.

2. The apparatus for producing terpene phenol resin according to claim 1, characterized in that, The height of the first receiver is higher than the height of the reactor.

3. The apparatus for producing terpene phenol resin according to claim 1, characterized in that, The height of the second receiver is lower than the height of the reactor.

4. The apparatus for producing terpene phenol resin according to claim 3, characterized in that, The height of the oil-water separator is the same as the height of the second receiver.

5. The apparatus for producing terpene phenol resin according to claim 1, characterized in that, The height of the phenol storage tank is higher than the height of the reaction vessel.

6. The apparatus for producing terpene phenol resin according to claim 1, characterized in that, It also includes a circulation balancing pipe, the beginning of which is connected to the upper part of the first receiver and the end of which is connected to the inclined descending section of the first pipe.

7. A method for producing terpene phenol resin, characterized in that, Based on the production apparatus for terpene phenol resin according to any one of claims 1 to 6, the production method includes the following steps: S1: Inputting the reaction raw materials into the reaction vessel, including metering the phenol from the phenol storage tank into the reaction vessel; S2: Control the continuous heating of the reactor. When the temperature inside the reactor is in the range of 150-250℃, the first, second, third, fourth, fifth, and sixth electric control valves are closed, and the seventh electric control valve is opened, so that the first receiver is in a negative pressure vacuum state. The first receiver is connected to the reactor, forming a suction effect, so that the gaseous phenol in the reactor is cooled into liquid through the first pipe and enters the first receiver. S3: When the temperature inside the reactor reaches 250℃, maintain the temperature at 250℃, control the first solenoid valve to open, so that the second receiver and the first receiver are both in a negative pressure state; after a preset time, control the fourth solenoid valve to open, so that the phenol collected in the first receiver is discharged to the second receiver by gravity; after a preset time, control the fourth solenoid valve to close. S4: The reactor continues to heat up to 270°C and maintains the temperature at 270°C. During this period, the second and third electric control valves are opened, so that part of the high-boiling-point heavy oil vapor in the reactor is condensed through the first pipe and enters the first receiver from the top, while the other part enters the first receiver from the bottom through the third pipe. S5: The reactor discharges and samples every 2 hours to test the degree of reaction of the product. Once the product reaches the predetermined degree of reaction, the reactor stops heating and discharges the product. At the same time, the fifth electric control valve is opened to allow the high-boiling-point heavy oil in the first receiver to enter the oil-water separator for processing through the third pipeline.

8. The method for producing terpene phenol resin according to claim 7, characterized in that, S4 also includes: controlling the opening of the sixth solenoid valve and controlling the opening of the material pump, so that the phenol in the second receiver is pumped into the phenol storage tank.

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