Aramid adhesive preparation neutralization reactor, production system and preparation process

Abstract

This invention discloses a neutralization reactor, production system, and preparation process for aramid adhesives. The neutralization reactor is a multi-stage continuous mixing reactor. The interior of the shell, from top to bottom, is equipped with a resin dispersion disc, a primary dispersion chamber, a secondary dispersion chamber, a tertiary dispersion chamber, and a discharge chamber. A rotating shaft is located at the bottom of the shell from bottom to top. The production system includes a solvent storage tank, a polymerization reactor, a neutralization reactor, a neutralization product buffer tank, a filter, and a product buffer tank, connected in sequence. The resin neutralization reactor of this invention employs multi-stage dispersion and high-shear reaction, greatly increasing the gas-liquid contact area, significantly improving the reaction rate, achieving near 100% neutralizer utilization, eliminating waste, and reducing tail gas recovery costs, thus lowering production costs. The production system of this invention effectively solves the problem of low production efficiency in aramid adhesives, providing an effective and feasible solution for mass production.

Description

Technical Field

[0001] This invention belongs to the field of adhesive technology, and particularly relates to a neutralization reactor, production system and preparation process for preparing aramid adhesives. Background Technology

[0002] Aramid adhesive is an adhesive based on meta-aramid resin, which has good adhesion and durability. It is particularly strong for bonding aramid paper, aramid paper to board, and aramid board. It is mainly used for bonding the ends of aramid paperboard in transformers and motors to ensure the stability of its insulation structure. Therefore, it is widely used in high-speed trains, aerospace, defense, electronics and other fields.

[0003] Currently, there are two methods for preparing aramid adhesives. One method involves interfacial polymerization, where the obtained solid polymer is dried and then dissolved to a certain concentration to prepare the adhesive product. This method suffers from difficulties in controlling the degree of polymerization, resulting in poor stability and a low yield. The other method uses low-temperature solution polycondensation, where the resulting polymer undergoes neutralization, desalination, and viscosity adjustment to prepare the aramid adhesive. Traditional batch reactors, due to their small aspect ratio and small gas-liquid reaction contact area, severely limit the reaction rate and result in low efficiency. During the reaction, some ammonia gas fails to react in time and is discharged from the reactor, causing waste and increasing tail gas treatment costs. This phenomenon becomes more pronounced the larger the batch reactor, thus significantly limiting the mass production of aramid adhesives. In particular, during the neutralization reaction, the small contact area between the neutralizing agent and the polymer solution and the low reaction rate lead to extremely low utilization efficiency of the neutralizing agent. Summary of the Invention

[0004] To overcome the problems in the prior art, the present invention provides a neutralization reactor, production system and preparation process for the preparation of aramid adhesives. The prepared neutralization reactor adopts multi-stage dispersion and high shear reaction, which greatly increases the gas-liquid contact area, greatly improves the reaction rate, and achieves a neutralizing agent utilization rate of nearly 100%. There is no waste and no increase in tail gas recovery costs, thus reducing production costs.

[0005] To solve the above-mentioned technical problems, the present invention proposes the following technical solution:

[0006] This invention provides a neutralization reactor for the preparation of aramid adhesives. The neutralization reactor is a multi-stage continuous mixing neutralization reactor, including a shell. The shell contains, from top to bottom, a resin dispersion disc, a primary dispersion chamber, a secondary dispersion chamber, a tertiary dispersion chamber, and a discharge chamber. A rotating shaft is provided at the bottom of the shell from bottom to top.

[0007] The resin dispersion disc is connected to the housing, and the resin dispersion disc is uniformly provided with several small holes; the primary dispersion chamber is provided with a stirring rotor fixedly connected to the rotating shaft in the center, and the housing of the primary dispersion chamber is provided with an air inlet; the secondary dispersion chamber and the tertiary dispersion chamber are each provided with a rotor disc and a stator disc, the rotor disc is fixed on the rotating shaft, the stator disc is fixedly connected to the housing, the stator disc and the rotor disc are provided with several protruding structures, and a gap is formed between two adjacent protruding structures. The protruding structures and gaps on the stator disc and the rotor disc are staggered, and the protruding structures extend into the gaps and are separated from the bottom of the gaps.

[0008] In this invention, after the resin solution enters the neutralization reactor from the top, it flows evenly down through small holes in the resin dispersion disc to prevent resin clumps from forming. After the resin enters the primary dispersion chamber evenly, the neutralizing agent ammonia is uniformly dispersed with the resin. Then, it passes through the secondary and tertiary dispersion chambers, allowing the neutralizing agent to fully react with the hydrogen chloride in the resin, thus achieving the neutralization effect. The secondary and tertiary dispersion chambers in this invention are configured as rotor and stator discs, with staggered protrusions on the rotor and stator discs. When the rotor disc moves with the rotating shaft, it drives the resin to move, which enhances mass transfer, accelerates the reaction, and allows the reaction to be more complete within a short residence time.

[0009] As an optional implementation, in the neutralization reactor provided by the present invention, the primary dispersion chamber is provided with a plurality of air inlets, and the air inlets are provided with check valve devices.

[0010] In this invention, an air inlet is provided on the primary dispersion chamber, and ammonia gas is injected through the air inlet to neutralize the polymer solution.

[0011] As an optional implementation, in the neutralization reactor provided by the present invention, the gap between the protrusions on the stator disk and the protrusions on the rotor disk in the secondary dispersion chamber is greater than the gap between the protrusions on the stator disk and the protrusions on the rotor disk in the tertiary dispersion chamber.

[0012] The gap between the protrusions on the stator disk and the protrusions on the rotor disk in the secondary dispersion chamber is larger than the gap in the secondary dispersion chamber. The reason is that as the neutralization reaction proceeds, more ammonium chloride salt is generated. As ammonium chloride becomes insoluble in the resin system, the mobile phase becomes worse. To ensure smooth flow and consistent flow rate, the tertiary dispersion interval should be larger than the secondary dispersion gap, specifically 5~10 mm.

[0013] As an optional implementation, in the neutralization reactor provided by the present invention, the gap between the protrusions on the stator disk and the protrusions on the rotor disk in the secondary dispersion chamber is 3~8 mm, and the gap between the protrusions on the stator disk and the protrusions on the rotor disk in the tertiary dispersion chamber is 5~10 mm.

[0014] In this invention, the gap between the raised structures on the stator disk and the raised structures on the rotor disk in the secondary dispersion chamber is set to 3-8 mm. This facilitates a full reaction while ensuring the first-in, first-out (FIFO) flow of the resin. If the gap is set too large, it will affect the resin delivery effect, causing the neutralizing agent and hydrogen chloride in the resin to not react fully.

[0015] As an optional implementation, in the neutralization reactor provided by the present invention, the distance between two adjacent protrusions on the stator disk or rotor disk in the secondary dispersion chamber is 26~36 mm, and the distance between two adjacent protrusions on the stator disk or rotor disk in the tertiary dispersion chamber is 30~40 mm.

[0016] As an optional implementation, in the neutralization reactor provided by the present invention, the shell is provided with a jacket, and a refrigerant is introduced into the jacket.

[0017] In this invention, the neutralization reaction is an exothermic process, and the high-speed stirring of the rotor will generate heat through friction. The high-temperature product will turn yellow, so a jacketed refrigerant is needed to remove the heat.

[0018] As an optional implementation, in the neutralization reactor provided by the present invention, an online pH meter is provided in the discharge chamber.

[0019] In this invention, during neutralization, in order to ensure that the acidic substance hydrogen chloride is completely neutralized, and at the same time, the alkali should not be excessive, as excessive alkalinity will also affect the performance of the product, the pH value of the resin is detected by an online pH meter in the discharge chamber.

[0020] Based on the same technical concept, the present invention also provides a production system for preparing aramid adhesives, comprising a solvent storage tank, a polymerization reactor, the aforementioned neutralization reactor, a neutralization product buffer tank, a filter, and a product buffer tank connected in sequence; the polymerization reactor includes polymerization reactor A and polymerization reactor B, which are connected in parallel, and the outlets of both polymerization reactor A and polymerization reactor B are connected to the inlet of the neutralization reactor; the product buffer tank includes product buffer tank A and product buffer tank B, which are connected in parallel, and the outlet of the filter is connected to both product buffer tank A and product buffer tank B.

[0021] In this invention, in order to achieve continuous production of aramid adhesive, two polymerization reactors and two product storage tanks are set up in parallel.

[0022] As an optional implementation, in the production system provided by the present invention, the product buffer tank is provided with an air inlet at the bottom and an exhaust outlet at the top. The air inlet is connected to a nitrogen storage tank, and the exhaust outlet is connected to a waste gas absorption device.

[0023] This invention incorporates a nitrogen bubbling device in the product buffer tank, which reduces the ammonia odor in the product and solves the problem of strong odor in aramid adhesives.

[0024] As an optional implementation, the production system provided by the present invention further includes a neutralizing agent storage tank, the outlet of which is connected to the inlet of the neutralizing reactor, and a rotor pump is provided between the polymerization reactor and the neutralizing reactor, and between the neutralization product buffer tank and the filter.

[0025] As an optional implementation, in the production system provided by the present invention, a mass flow meter is provided on the pipeline connecting the discharge port of the polymerization reactor and the neutralization reactor.

[0026] As an optional implementation, in the production system provided by the present invention, a mass flow meter is provided on the pipeline connecting the outlet of the neutralizing agent storage tank to the neutralization reactor.

[0027] As an optional implementation, in the production system provided by the present invention, the discharge port of the polymerization reactor is connected to the neutralization reactor via a rotor pump.

[0028] As an optional implementation, in the production system provided by the present invention, the outlet of the neutralization product buffer tank is connected to a filter via a rotor pump.

[0029] Based on the same technical concept, the present invention also provides a preparation process for an aramid adhesive, comprising the following steps:

[0030] S1. Under a nitrogen atmosphere, organic solvent and m-phenylenediamine are added to the polymerization reactor. After cooling to -15~-5℃, isophthaloyl chloride is slowly added in an equimolar ratio to obtain a polymer solution. The obtained polymer solution is diluted to a certain concentration for later use.

[0031] S2. Start the neutralization reactor and feed the polymer solution obtained in step S1 and the neutralizing agent into the neutralization reactor at a certain flow rate for neutralization reaction. The motor speed of the neutralization reactor is 100~1000r / min. The online pH meter in the discharge chamber monitors the pH value in real time and controls it at 7~7.5. The neutralization temperature is controlled at 20~30℃. The material coming out of the neutralization reactor directly enters the intermediate product buffer tank.

[0032] S3. The material in the intermediate product buffer tank in step S2 is transported to the filter for filtration and desalination. The filtered clear liquid is directly fed into the product buffer tank.

[0033] S4. Turn on the stirring motor of the product buffer tank and introduce nitrogen into the product buffer tank from the bottom at a certain flow rate. Use bubbling to discharge the small amount of neutralizing agent in the product.

[0034] In this invention, the high solid content in the polymerization reaction of intermediate-phenylenediamine and isophthaloyl chloride in step S1 leads to a high apparent viscosity. Therefore, the resulting polymer solution is diluted to facilitate feeding, neutralization reaction, and subsequent filtration. In the neutralization reactor, the neutralizing agent ammonia reacts with hydrogen chloride in the polymer to generate ammonium chloride solid, which is then separated by filtration. Since hydrogen chloride is a strong acid, it affects the performance of the product and must be removed. During neutralization, to ensure that the acidic hydrogen chloride is completely neutralized, while also preventing excessive alkali (which also affects product performance), the pH value of the resin is monitored by an online pH meter in the discharge chamber and needs to be controlled within the range of 7-7.5.

[0035] As an optional implementation, in the preparation process provided by the present invention, in step S1, the obtained polymer solution is diluted to a concentration of 8% to 12%, and the apparent viscosity of the diluted polymer solution is controlled at 500 to 1000 centipoise.

[0036] As an optional implementation, in the preparation process provided by the present invention, in step S2, the neutralizing agent is ammonia, the flow rate of the neutralizing agent is 10~60 g / min, and the flow rate of the polymer solution is 1000~4000 g / min.

[0037] As an optional implementation, in the preparation process provided by the present invention, in step S4, the nitrogen inlet gas flow rate is 5~10m. 3 / h, bubbling time is 1~2h.

[0038] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0039] This invention provides a highly efficient and continuous apparatus and process for preparing aramid adhesives. In particular, it offers a resin neutralization reactor that employs multi-stage dispersion and high-shear reaction, significantly increasing the gas-liquid contact area and greatly improving the reaction rate. The neutralizer utilization rate is close to 100%, with no waste and no additional tail gas recovery costs, thus reducing production costs. A nitrogen bubbling step is added to the production system and preparation process to reduce the ammonia odor in the product. This effectively solves the problems of low production efficiency, significant neutralizer waste, and strong odor in aramid adhesives, providing an effective and feasible solution for mass production. Attached Figure Description

[0040] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0041] Figure 1 This is a schematic diagram of the neutralization reactor in Embodiment 1 of the present invention;

[0042] Figure 2 This is a schematic diagram of the stator disk structure in Embodiment 1 of the present invention;

[0043] Figure 3 This is a schematic diagram of the rotor disk structure in Embodiment 1 of the present invention;

[0044] Figure 4 This is a schematic diagram of the production system for preparing aramid adhesive in Embodiment 2 of the present invention.

[0045] Figure label:

[0046] 1. Solvent storage tank; 2. Polymerization reactor; 4. First rotor pump; 5. Neutralizing agent storage tank; 6. Neutralization reactor; 7. Neutralization product buffer tank; 8. Second rotor pump; 9. Filter; 10. Product buffer tank;

[0047] 6-1. Shell; 6-2. Jacket; 6-3. Resin dispersion disc; 6-4. Primary dispersion chamber; 6-5. Secondary dispersion chamber; 6-6. Tertiary dispersion chamber; 6-7. Discharge chamber; 6-8. Air inlet; 6-9. Stirring rotor; 6-10. Stator disc; 6-11. Rotor disc; 6-12. Online pH meter; 6-13. Rotating shaft; 6-14. Raised structure. Detailed Implementation

[0048] To facilitate understanding of the present invention, the present invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of protection of the present invention is not limited to the following specific embodiments.

[0049] Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by those skilled in the art. The technical terms used herein are for the purpose of describing particular embodiments only and are not intended to limit the scope of the invention.

[0050] Unless otherwise specified, all raw materials, reagents, instruments and equipment used in this invention can be purchased from the market or prepared by existing methods.

[0051] Example 1

[0052] A neutralization reactor for the preparation of aramid adhesives, the structural schematic diagram of which is shown below. Figure 1 As shown, the neutralization reactor 6 is a multi-stage continuous mixing neutralization reactor, including an outer shell 6-1. Inside the shell 6-1, from top to bottom, there are resin dispersion discs 6-3, primary dispersion chamber 6-4, secondary dispersion chamber 6-5, tertiary dispersion chamber 6-6, and discharge chamber 6-7. A rotating shaft 6-13 is arranged from bottom to top at the bottom of the shell 6-1. The rotating shaft 6-13 is located at the bottom of the discharge chamber 6-7 and passes through the tertiary dispersion chamber 6-6, secondary dispersion chamber 6-5, and primary dispersion chamber 6-4 in sequence.

[0053] The resin dispersion disk 6-3 is connected to the shell 6-1. Several small holes are evenly arranged on the resin dispersion disk 6-3. Specifically, the resin dispersion disk 6-3 is circular and has several small holes for the polymer solution entering from the top to flow down into the lower primary dispersion chamber 6-4.

[0054] After the polymer solution flows down from the resin dispersion plate 6-3, it enters the primary dispersion chamber 6-4. The primary dispersion chamber 6-4 is provided with a stirring rotor 6-9 fixedly connected to the rotating shaft 6-13 in the center. The housing 6-1 of the primary dispersion chamber 6-4 is provided with an air inlet 6-8, and the air inlet 6-8 is provided with a check valve device.

[0055] In this application, the upper end of the rotating shaft 6-13 enters the primary dispersion chamber 6-4, and the upper part is fixedly connected to the stirring rotor 6-9. When the rotating shaft 6-13 is started, it drives the stirring rotor 6-9 to rotate. At this time, the polymer solution entering the primary dispersion chamber 6-4 is stirred under the action of the stirring rotor 6-9. Simultaneously, an air inlet 6-8 is provided on the side wall of the primary dispersion chamber 6-4 shell for spraying in a neutralizing agent to neutralize the polymer solution. A backflow preventer is provided to prevent the neutralizing agent from flowing back. In the preparation of aramid adhesive, ammonia is used as the neutralizing agent. Introducing ammonia during stirring increases the contact area between the ammonia and the polymer solution, thereby increasing the utilization rate of the neutralizing agent.

[0056] After passing through the primary dispersion chamber 6-4, the polymer solution enters the secondary dispersion chamber 6-5. The secondary dispersion chamber 6-5 is equipped with a rotor disk 6-11 and a stator disk 6-10, as shown in the schematic diagram below. Figure 2 and 3As shown, the rotor disk 6-11 is fixed to the rotating shaft 6-13, and the stator disk 6-10 is fixed to the housing 6-1. Several protruding structures 6-14 are provided on both the stator disk 6-10 and the rotor disk 6-11, with gaps between adjacent protruding structures 6-14. The protruding structures 6-14 on the stator disk 6-10 and the rotor disk 6-11 are staggered, extending into the gaps and separated from the bottom of the gaps. In this application, the stator disk 6-10 is positioned above the rotor disk 6-11, with one end fixed to the housing and the other end suspended. Several protruding structures 6-14 are provided on the lower surface of the stator disk 6-10, with gaps between adjacent protruding structures 6-14, as detailed below. Figure 2 As shown, the protruding structures 6-14 are arranged in a ring shape. The rotor disk 6-11, located below the stator disk 6-10, is fixed at one end to the rotating shaft and suspended at the other end. The protruding structures 6-14 on the rotor disk 6-11 are arranged in the same manner as those on the stator disk 6-10, as shown below. Figure 3 As shown, in the specific configuration, the protrusions 6-14 on the stator disk 6-10 and the gaps on the rotor disk 6-11 are arranged in an intersecting manner. That is, the protrusions 6-14 on the stator disk 6-10 extend into the gaps on the rotor disk 6-11, and the protrusions 6-14 on the rotor disk 6-11 extend into the gaps on the stator disk 6-10. However, the protrusions 6-14 extend into the gaps and are separated from the bottom of the gaps, meaning that the two do not contact each other.

[0057] After passing through the secondary dispersion chamber 6-5, the polymer solution enters the tertiary dispersion chamber 6-6. The structure of the tertiary dispersion chamber 6-6 is the same as that of the secondary dispersion chamber 6-5. The difference is that the gap between the protrusions 6-14 on the stator disk 6-10 and the protrusions 6-14 on the rotor disk 6-11 in the secondary dispersion chamber 6-5 is larger than the gap between the protrusions 6-14 on the stator disk 6-10 and the protrusions 6-14 on the rotor disk 6-11 in the tertiary dispersion chamber 6-6. Specifically, the gap between the protrusions 6-14 on the stator disk and the protrusions 6-14 on the rotor disk in the secondary dispersion chamber 6-5 is 3~8mm, while the gap between the protrusions 6-14 on the stator disk and the protrusions 6-14 on the rotor disk in the tertiary dispersion chamber 6-6 is 5~10mm.

[0058] In the secondary dispersion cavity 6-5, the distance between two adjacent protrusions 6-14 on the stator disk 6-10 or rotor disk 6-11 is 26~36 mm, and in the tertiary dispersion cavity 6-6, the distance between two adjacent protrusions 6-14 on the stator disk 6-10 or rotor disk 6-11 is 30~40 mm.

[0059] After passing through the three-stage dispersion chamber 6-6, the polymer solution is discharged from the bottom discharge chamber 6-7. The discharge chamber 6-7 is equipped with an online pH meter 6-12 for real-time detection of the pH value of the polymer solution.

[0060] In this application, the shell 6-1 is provided with a jacket 6-2, and a refrigerant is introduced into the jacket 6-2, specifically cold water. In this embodiment, the water inlet is located at the bottom of the neutralization reactor, and the water outlet is located at the top of the neutralization reactor.

[0061] like Figure 1 As shown, the polymer solution flows in the neutralization reactor in the direction indicated by the arrow to complete the neutralization reaction process.

[0062] Example 2

[0063] A production system for preparing aramid adhesives, the structural schematic diagram of which is shown below. Figure 4 As shown, it includes a solvent storage tank 1, a polymerization reactor 2, a neutralization reactor 6 (as in Example 1), a neutralization product buffer tank 7, a filter 9, and a product buffer tank 10, which are connected in sequence.

[0064] Polymerization reactor 2 includes polymerization reactor A and polymerization reactor B, which are connected in parallel. The outlets of both polymerization reactors A and B are connected to the inlet of neutralization reactor 6. In this embodiment, polymerization reactor 2 is an enamel-lined kettle with a jacket and a stirring device. The jacket can be filled with both heat and cold media. The stirring motors are variable frequency motors that can display current and torque values, and the stirring paddles are PTFE-lined double-ribbed stirrers.

[0065] The polymer solution obtained after the polymerization reaction is connected to the neutralization reactor 6 via the outlets of polymerization reactors A and B through the first rotor pump 4. A mass flow meter is also installed on the pipeline connecting polymerization reactors 2 and neutralization reactor 6. The structure of neutralization reactor 6 is the same as in Example 1. A neutralizing agent storage tank 5 is also connected to the air inlet of neutralization reactor 6 for storing the neutralizing agent.

[0066] After passing through the neutralization reactor 6, the polymer solution is discharged from the discharge chamber and enters the neutralization product buffer tank 7, and then, after metering, enters the filter 9. In this application, the discharge port of the neutralization product buffer tank 7 is connected to the filter 9 through a second rotor pump 8, and a mass flow meter is also installed on the connected pipeline.

[0067] In this embodiment only, filter 9 is a plate and frame filter with a filtration accuracy of 5μm and a filtration area depending on the production capacity. Specifically, two or more plate and frame filters can be used in parallel according to the actual usage.

[0068] After filtration and desalination, the polymer solution enters the product buffer tank 10. In this application, two product buffer tanks are provided, including product buffer tank A and product buffer tank B, which are connected in parallel. Both product buffer tanks 10 have air inlets at the bottom and exhaust outlets at the top. The air inlets are connected to a nitrogen storage tank, and the exhaust outlets are connected to a waste gas absorption device. The nitrogen bubbling process can reduce the ammonia odor of the product.

[0069] Example 3

[0070] A process for preparing an aramid adhesive includes the following steps:

[0071] (1) Under a nitrogen atmosphere, 20 kg of m-phenylenediamine and 200 kg of DMAc were added to a 300 L polymerization reactor. After stirring and dissolving, the jacket cooling was turned on to lower the temperature to -10 °C. Then, 37.6 kg of isophthaloyl chloride was slowly added in batches. As the isophthaloyl chloride feed rate approached 100%, the polymer viscosity increased. When the viscosity reached 80,000 centipoise, the feed was stopped. Then, 183 kg of DMAC was added and stirred for 10 min to dilute the resin to a concentration of 10%. The apparent viscosity was measured to be 900 centipoise. The next step was then carried out.

[0072] (2) Start the neutralization reactor and transport the polymer solution obtained in step (1) and the neutralizing agent to the neutralization reactor for neutralization reaction. The flow rate of the polymer solution is 1000~4000 g / min, the flow rate of the neutralizing agent ammonia is 10~60 g / min, the motor speed of the neutralization reactor is 100~1000 r / min, the online pH meter in the discharge chamber is monitored in real time, and the pH value is controlled between 7 and 7.5. The neutralization temperature is controlled at about 20~30℃. The material coming out of the neutralization reactor directly enters the intermediate product buffer tank.

[0073] (3) The material in the intermediate product buffer tank in step (2) is transported to the filter for filtration and desalination, and the filtered clear liquid is directly fed into the product buffer tank.

[0074] (4) Turn on the stirring motor of the product buffer tank and purge nitrogen at a rate of 5~10m. 3 A flow rate of / h is introduced from the bottom into the buffer tank, and a small amount of neutralizing agent in the product is discharged by bubbling.

[0075] The above description, in conjunction with specific preferred embodiments, provides a further detailed explanation of the present invention. However, it should not be construed that the specific implementation of the present invention is limited to these descriptions. For those skilled in the art, various simple deductions or substitutions can be made without departing from the concept of the present invention, and all such modifications and substitutions should be considered within the scope of protection of the present invention.

Claims

1. An aramid adhesive preparation neutralization reactor, characterized by, The neutralization reactor (6) is a multi-stage mixing continuous neutralization reactor, including a shell (6-1). The shell (6-1) is provided with a resin dispersion plate (6-3), a primary dispersion chamber (6-4), a secondary dispersion chamber (6-5), a tertiary dispersion chamber (6-6), and a discharge chamber (6-7) from top to bottom. A rotating shaft (6-13) is provided at the bottom of the shell (6-1) from bottom to top. The resin dispersion disc (6-3) is connected to the housing (6-1), and the resin dispersion disc (6-3) is evenly provided with several small holes; the primary dispersion chamber (6-4) has a stirring rotor fixedly connected to the rotating shaft (6-13) in the center, and the housing of the primary dispersion chamber (6-4) is provided with several air inlets (6-8), and the air inlets (6-8) are provided with check valve devices; the secondary dispersion chamber (6-5) and the tertiary dispersion chamber (6-6) are both provided with rotor disc (6-11) and stator disc (6-11). -10), the rotor disk (6-11) is fixed on the rotating shaft (6-13), the stator disk (6-10) is fixed on the housing (6-1), the stator disk (6-10) and the rotor disk (6-11) are provided with a plurality of protruding structures (6-14), a gap is formed between two adjacent protruding structures (6-14), the protruding structures (6-14) on the stator disk (6-10) and the rotor disk (6-11) are staggered, and the protruding structures (6-14) extend into the gap and are separated from the bottom of the gap; The gap between the protruding structure (6-14) on the stator disk (6-10) and the protruding structure (6-14) on the rotor disk (6-11) in the secondary dispersion cavity (6-5) is greater than the gap between the protruding structure (6-14) on the stator disk (6-10) and the protruding structure (6-14) on the rotor disk (6-11) in the tertiary dispersion cavity (6-6). The housing (6-1) is provided with a jacket (6-2), and refrigerant is introduced into the jacket (6-2).

2. The neutralization reactor for preparing aramid adhesives according to claim 1, characterized in that, An online pH meter is installed inside the discharge chamber.

3. A production system for preparing aramid adhesives, characterized in that, The system comprises a solvent storage tank (1), a polymerization reactor (2), a neutralization reactor (6) as described in claim 2, a neutralization product buffer tank (7), a filter (9), and a product buffer tank (10) connected in sequence. The polymerization reactor (2) includes polymerization reactor A and polymerization reactor B, which are connected in parallel. The outlets of polymerization reactor A and polymerization reactor B are both connected to the inlet of neutralization reactor (6). The product buffer tank (10) includes product buffer tank A and product buffer tank B, which are connected in parallel. The outlet of the filter (9) is connected to both product buffer tank A and product buffer tank B.

4. The production system for preparing aramid adhesives according to claim 3, characterized in that, The product buffer tank (10) has an air inlet at the bottom and an exhaust outlet at the top. The air inlet is connected to a nitrogen storage tank, and the exhaust outlet is connected to a waste gas absorption device.

5. The production system for preparing aramid adhesives according to claim 4, characterized in that, The production system also includes a neutralizing agent storage tank (5), the outlet of which is connected to the inlet of the neutralizing reactor (6), and a rotor pump is provided between the polymerization reactor (2) and the neutralizing reactor (6), and between the neutralization product buffer tank (7) and the filter (9).

6. A preparation process for an aramid adhesive, characterized in that, The preparation process is applied to the production system for preparing aramid adhesives according to claim 5, and includes the following steps: S1. Under a nitrogen atmosphere, organic solvent and m-phenylenediamine are added to a polymerization reactor. After cooling to -15~-5℃, isophthaloyl chloride is slowly added in an equimolar ratio to react and obtain a polymer solution. The obtained polymer solution is diluted to a certain concentration for later use. S2. Start the neutralization reactor and feed the polymer solution obtained in step S1 and the neutralizing agent into the neutralization reactor at a certain flow rate for neutralization reaction. The motor speed of the neutralization reactor is 100~1000r / min. The online pH meter in the discharge chamber monitors the pH value in real time and controls it at 7~7.

5. The neutralization temperature is controlled at 20~30℃. The material coming out of the neutralization reactor directly enters the neutralization product buffer tank. S3. The material in the neutralization product buffer tank in step S2 is transported to the filter for filtration and desalination. The filtered clear liquid is directly introduced into the product buffer tank. S4. Turn on the stirring motor of the product buffer tank and introduce nitrogen into the product buffer tank from the bottom at a certain flow rate. Use bubbling to discharge the small amount of neutralizing agent in the product.

7. The preparation process of the aramid adhesive according to claim 6, characterized in that, In step S1, the obtained polymer solution is diluted to a concentration of 8% to 12%, and the apparent viscosity of the diluted polymer solution is controlled at 500 to 1000 centipoise.

8. The preparation process of the aramid adhesive according to claim 6, characterized in that, In step S2, the neutralizing agent is ammonia, the flow rate of the neutralizing agent is 10~60 g / min, and the flow rate of the polymer solution is 1000~4000 g / min.

9. The preparation process of the aramid adhesive according to claim 6, characterized in that, In step S4, the nitrogen gas flow rate is 5-10 m 3 / h, and the bubbling time is 1-2 h.

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