Double-temperature-control reaction kettle and preparation method of ultrahigh-viscosity polymer binder

Abstract

The invention discloses a dual-temperature-control reaction kettle and a preparation method of an ultrahigh-viscosity polymer binder, and relates to the technical field of reaction kettles, the dual-temperature-control reaction kettle comprises a reaction kettle body, a metal supporting piece, a reaction kettle jacket, a temperature adjusting mechanism and a temperature controller. The reaction kettle body sinks towards the inner center to form a mounting groove and is provided with a metal supporting piece, the temperature of the inner center of the reaction kettle body can be detected, and the temperature controller adjusts the temperature of the temperature control medium in real time based on the detected temperature and exchanges heat with the reaction kettle jacket. Compared with the prior art, the central temperature of the reaction kettle can be accurately mastered so as to correspondingly adjust the temperature of the temperature control medium, on one hand, heat generated during high-molecular polymerization can be quickly conducted out when the temperature of the reaction kettle is too high, and the implosion phenomenon caused by polymerization reaction overexcitation is effectively prevented; on the other hand, insufficient temperature caused by excessive heat dissipation of the reaction kettle can be avoided, and the temperature of the reaction kettle can be rapidly and accurately controlled.

Description

Technical Field

[0001] The present invention relates to the technical field of reaction kettles, and particularly to a double-temperature-controlled reaction kettle and a preparation method of an ultra-high-viscosity polymer binder. Background Art

[0002] A reaction kettle is a chemical synthesis reaction vessel. In various chemical reactions, the reactions related to polymer synthesis have the following requirements for the reaction kettle:

[0003] 1. It is required that the temperature of the material in the reaction kettle is kept constant within the range of the target temperature ±0.5°C or less, and it is also required that the reaction kettle can adjust the temperature as quickly as possible and reach the optimal reaction temperature rapidly.

[0004] 2. It is required that the reaction kettle can quickly mix and contact the reaction materials sufficiently, so as to obtain the best reaction rate.

[0005] However, the existing reaction kettles do not have the function of quickly and accurately adjusting the temperature, and the stirring uniformity of the materials often fails to meet the requirements, thus being unable to adapt to the polymer synthesis reaction.

[0006] In view of this, how to provide a reaction kettle that can quickly and accurately adjust the temperature and can stir the materials sufficiently is an urgent problem to be solved by those skilled in the art. Summary of the Invention

[0007] The purpose of the present invention is to provide a double-temperature-controlled reaction kettle and a preparation method of an ultra-high-viscosity polymer binder to solve the problems existing in the prior art.

[0008] To achieve the above purpose, the present invention provides a double-temperature-controlled reaction kettle, including:

[0009] A reaction kettle body, the top of which is recessed towards the center inside the reaction kettle body to form an installation groove;

[0010] A metal support member, which is arranged in the installation groove, and the metal support member has a temperature measurement probe for detecting the temperature at the center inside the reaction kettle body;

[0011] A reaction kettle jacket, which is arranged on the outer surface of the reaction kettle body, and the reaction kettle jacket in the installation groove is located between the metal support member and the inner side wall of the installation groove;

[0012] A temperature adjustment mechanism, which can exchange heat with the reaction kettle jacket;

[0013] A temperature controller, the temperature measurement probe uploads the detected temperature data of the center inside the reaction kettle body to the temperature controller, and the temperature controller controls the temperature adjustment mechanism to exchange heat with the reaction kettle jacket.

[0014] Furthermore, the temperature adjustment mechanism comprises:

[0015] A temperature regulating medium storage tank is filled with a temperature controlling medium. A jacket chamber is defined inside the reactor jacket. A temperature controlling medium inlet and a temperature controlling medium outlet are provided on the reactor jacket and are connected to the jacket chamber. The temperature regulating medium storage tank is connected to the temperature controlling medium inlet and the temperature controlling medium outlet respectively.

[0016] A circulation pump, used to drive the temperature control medium to circulate between the jacket chamber and the temperature control medium storage tank;

[0017] The medium temperature regulating mechanism is electrically connected to the temperature controller. The temperature controller regulates the temperature of the temperature-controlled medium through the medium temperature regulating mechanism and exchanges heat with the jacket of the reactor.

[0018] Furthermore, it also includes:

[0019] A stirring shaft is rotatably disposed in the reactor body along a vertical direction and is connected to the stirring mechanism;

[0020] A servo motor, wherein the stirring shaft extends beyond the reactor body and is drivingly connected to the servo motor.

[0021] Furthermore, the servo motor is a variable frequency motor, and the stirring mechanism is a frame-type stirring paddle.

[0022] Furthermore, an annular reaction chamber is formed between the reactor body and the mounting groove, and the frame-type stirring paddle is arranged in the annular reaction chamber and extends upward.

[0023] Furthermore, at least two feed inlets are provided on the top of the reactor body, and the feed inlets are arranged on the left and right sides of the mounting groove and communicated with the annular reaction chamber.

[0024] Furthermore, a discharge port is provided at the bottom of the reactor body, the discharge port is connected to a discharge pipe, and a filter is provided at the port of the discharge pipe.

[0025] Furthermore, the discharge pipe is connected to the discharge screw pump.

[0026] Furthermore, it also includes a universal reactor bracket, and the reactor body is arranged on the universal reactor bracket.

[0027] The present invention also provides a method for preparing an ultra-high viscosity polymer adhesive, using a double temperature-controlled reactor, comprising the following steps:

[0028] S1: Mix carboxyl - terminated nitrile rubber, N - (3 - aminopropyl) methacrylamide, acrylonitrile, a catalyst and a non - ionic surfactant uniformly in water, and prepare a seed emulsion through reaction. The reaction time is 2 - 4 h, and the reaction temperature is 40 - 60 °C;

[0029] S2: Add an alkali solution to methacrylic acid to obtain a methacrylate solution;

[0030] S3: Add the methacrylate solution and non - polar monomers to the seed emulsion in sequence, and obtain a reaction emulsion after stirring evenly;

[0031] S4: Under an inert gas atmosphere, drop an initiator into the reaction emulsion for reaction. The reaction time is 8 - 12 h, and the reaction temperature is 40 - 90 °C; After cooling, perform degassing, dilution with water, and filtration in sequence to obtain an ultra - high - viscosity polymer binder.

[0032] The present invention discloses the following technical effects:

[0033] 1. The reaction kettle body is recessed towards the inner center to form an installation groove and a metal support is provided, which can detect the temperature at the center inside the reaction kettle body. The temperature controller adjusts the temperature of the temperature - control medium in real - time based on the detected temperature and exchanges heat with the reaction kettle jacket. Compared with the prior art, it can accurately master the temperature at the center of the reaction kettle and then correspondingly adjust the temperature of the temperature - control medium. On the one hand, when the temperature of the reaction kettle is too high, it can quickly export the heat generated during the polymerization of the polymer, effectively preventing the over - violent polymerization reaction from causing the phenomenon of explosive polymerization; on the other hand, it can also avoid excessive heat dissipation of the reaction kettle resulting in insufficient temperature, thereby achieving rapid and accurate control of the reaction kettle temperature.

[0034] 2. The servo motor is arranged at the bottom of the reaction kettle and is a variable - frequency motor, which shortens the length requirement of the stirring shaft, can provide a greater torque for the stirring paddle, and then quickly and evenly stir the materials in the reaction kettle.

[0035] 3. The stirring mechanism adopts a frame - type stirring paddle, which can reduce the friction between the paddle blades and the materials, and can not only stir conventional materials, but also quickly and evenly stir the reaction materials of the ultra - high - viscosity binder. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for use in the embodiments. Obviously, the following - described drawings are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0037] Figure 1 It is a schematic structural diagram of the present invention;

[0038] Among them, 1 is the feed inlet; 2 is the reaction kettle jacket; 3 is the jacket chamber; 4 is the reaction kettle body; 5 is the temperature control medium inlet; 6 is the universal reaction kettle support; 7 is the servo motor; 8 is the discharge outlet; 9 is the stirring shaft; 10 is the temperature control medium outlet; 11 is the frame type stirring paddle; 12 is the metal support. Specific embodiments

[0039] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present invention.

[0040] To make the above objects, features, and advantages of the present invention more obvious and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0041] The embodiment of the present invention provides a double-temperature control reaction kettle, including:

[0042] The reaction kettle body 4, the top of which is recessed towards the center of the inside of the reaction kettle body 4 to form an installation groove;

[0043] The metal support 12 is arranged in the installation groove. The metal support 12 has a temperature measurement probe for detecting the temperature at the center of the inside of the reaction kettle body 4;

[0044] The reaction kettle jacket 2 is arranged on the outer surface of the reaction kettle body 4. The reaction kettle jacket 2 in the installation groove is located between the metal support 12 and the inner side wall of the installation groove;

[0045] The temperature adjustment mechanism can exchange heat with the reaction kettle jacket 2;

[0046] The temperature controller. The temperature measurement probe uploads the detected temperature data at the center of the inside of the reaction kettle body 4 to the temperature controller, and the temperature controller controls the temperature adjustment mechanism to exchange heat with the reaction kettle jacket 2.

[0047] In this embodiment, the temperature adjustment mechanism includes:

[0048] The temperature adjustment medium storage tank is filled with a temperature control medium. A jacket chamber 3 is defined inside the reaction kettle jacket 2. The reaction kettle jacket 2 is provided with a temperature control medium inlet 5 and a temperature control medium outlet 10 communicating with the jacket chamber 3. The temperature adjustment medium storage tank is respectively communicated with the temperature control medium inlet 5 and the temperature control medium outlet 10;

[0049] The circulation pump is used to drive the temperature control medium to circulate between the jacket chamber 3 and the temperature adjustment medium storage tank;

[0050] A medium temperature regulating mechanism, which is electrically connected to a temperature controller. The temperature controller adjusts the temperature of the temperature control medium through the medium temperature regulating mechanism and exchanges heat with the jacket 2 of the reaction kettle. Both the temperature control medium and the medium temperature regulating mechanism can adopt existing technologies and will not be elaborated here.

[0051] In this embodiment, it further includes:

[0052] A stirring shaft 9, which is rotatably arranged vertically in the reaction kettle body 4 and is connected to a stirring mechanism;

[0053] A servo motor 7, and the stirring shaft 9 extends outside the reaction kettle body 4 and is in transmission connection with the servo motor 7.

[0054] In this embodiment, the servo motor 7 is a variable-frequency motor, and the stirring mechanism is a frame-type stirring paddle 11.

[0055] In this embodiment, an annular reaction chamber is formed between the reaction kettle body 4 and the installation groove, and the frame-type stirring paddle 11 is arranged in the annular reaction chamber and extends upward.

[0056] In this embodiment, at least two feed ports 1 are provided at the top of the reaction kettle body 4. The feed ports 1 are arranged on the left and right sides of the installation groove and are communicated with the annular reaction chamber.

[0057] In this embodiment, a discharge port 8 is provided at the bottom of the reaction kettle body 4. The discharge port 8 is communicated with a discharge pipe, and a 100-mesh filter screen is provided at the port of the discharge pipe.

[0058] In this embodiment, the discharge pipe is communicated with a discharge screw pump, which is convenient for rapid discharging.

[0059] In this embodiment, it further includes a universal reaction kettle support 6, and the reaction kettle body 4 is arranged on the universal reaction kettle support 6. The universal reaction kettle can rotate to adjust the center of gravity of the reaction kettle body 4, and thus it can be installed in different factories.

[0060] The present invention also provides a preparation method of an ultra-high viscosity polymer binder, which uses a dual-temperature-controlled reaction kettle and includes the following steps:

[0061] S1: Mix carboxyl-terminated nitrile rubber (8% of the total mass fraction), N-(3-aminopropyl) methacrylamide (17% of the total mass fraction), acrylonitrile (35% of the total mass fraction), 4-dimethylaminopyridine (1% of the mass fraction of carboxyl-terminated nitrile rubber), and a non-ionic surfactant (NP10, 2% of the mass fraction of carboxyl-terminated nitrile rubber) in water, stir vigorously (300 revolutions per minute) for 30 minutes, then heat to 50 °C, and allow the amino group in N-(3-aminopropyl) methacrylamide to fully react with the carboxyl group in carboxyl-terminated nitrile rubber for 3 h to prepare a partially acrylated carboxyl-terminated nitrile rubber (CTBN) seed emulsion, and cool to room temperature;

[0062] S2: Add an aqueous solution of sodium hydroxide (46.4% of the mass fraction of methacrylic acid) to (meth)acrylic acid (35% of the total mass fraction), and prepare a (meth)acrylate sodium salt solution through an acid-base neutralization reaction. Cool it to room temperature for standby.

[0063] S3: Sequentially add the (meth)acrylate sodium salt solution and butyl acrylate (5% of the total mass fraction) to the acrylated carboxyl-terminated butadiene acrylonitrile rubber (CTBN) seed emulsion solution prepared above, and vigorously stir (300 revolutions per minute) for 30 minutes to prepare an emulsion for reaction.

[0064] S4: Pass nitrogen for 30 minutes to remove oxygen in the reaction system, reduce the stirring speed (100 revolutions per minute), and after heating to 50 °C, gradually dropwise add an initiator (aqueous ammonium persulfate solution). Control the temperature at 50 °C and stir for 12 h. After cooling to room temperature, remove monomers, add water for dilution, and filter to obtain a polymer composite aqueous binder with a core-shell structure based on carboxyl-terminated butadiene acrylonitrile rubber (CTBN). Its specific parameters are: white latex, solid content of 8.0 wt% at 40 °C, pH value of 7.2, and viscosity of 24.2 Pa•s (adjust the solid content by adding water for dilution).

[0065] In the description of the present invention, it should be understood that the orientation or positional relationship indicated by the terms "longitudinal", "transverse", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. is based on the orientation or positional relationship shown in the drawings, and is only for the convenience of describing the present invention, 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 construed as a limitation to the present invention.

[0066] The embodiments described above are only for describing the preferred mode of the present invention, and do not limit the scope of the present invention. Without departing from the design spirit of the present invention, various deformations and improvements made by those of ordinary skill in the art to the technical solutions of the present invention shall fall within the protection scope determined by the claims of the present invention.

Claims

1. A double-temperature-controlled reaction kettle, characterized in that, Comprising: A reactor body (4), the top of which is recessed towards the center inside the reactor body (4) to form a mounting groove; A metal support (12) disposed in the mounting groove, the metal support (12) having a temperature measurement probe for detecting the temperature at the center inside the reactor body (4); A reactor jacket (2) disposed on the outer surface of the reactor body (4), and the reactor jacket (2) in the mounting groove is located between the metal support (12) and the inner side wall of the mounting groove; A temperature regulating mechanism capable of exchanging heat with the reactor jacket (2); A temperature controller, and the temperature measurement probe uploads the temperature data detected at the center inside the reactor body (4) to the temperature controller, and the temperature controller controls the temperature regulating mechanism to exchange heat with the reactor jacket (2).

2. The dual-temperature controlled reactor according to claim 1, wherein The temperature regulating mechanism includes: A temperature regulating medium storage tank filled with a temperature control medium. A jacket chamber (3) is defined inside the reactor jacket (2). A temperature control medium inlet (5) and a temperature control medium outlet (10) communicating with the jacket chamber (3) are provided on the reactor jacket (2), and the temperature regulating medium storage tank is respectively communicated with the temperature control medium inlet (5) and the temperature control medium outlet (10); A circulation pump for driving the temperature control medium to circulate between the jacket chamber (3) and the temperature regulating medium storage tank; A medium temperature regulating mechanism electrically connected to the temperature controller, and the temperature controller adjusts the temperature of the temperature control medium through the medium temperature regulating mechanism and exchanges heat with the reactor jacket (2).

3. The double-temperature-controlled reactor according to claim 2, wherein, Further comprising: A stirring shaft (9) rotatably disposed in the reactor body (4) in the vertical direction and connected to a stirring mechanism; A servo motor (7), and the stirring shaft (9) extends outside the reactor body (4) and is drivingly connected to the servo motor (7).

4. A dual-temperature controlled reactor according to claim 3, characterized in that, The servo motor (7) is a variable frequency motor, and the stirring mechanism is a frame type stirring paddle (11).

5. A double-temperature-controlled reactor according to claim 4, characterized in that, An annular reaction chamber is formed between the reactor body (4) and the mounting groove, and the frame type stirring paddle (11) is arranged in the annular reaction chamber and extends upward.

6. The dual-temperature controlled reactor according to claim 5, wherein, At least two feed ports (1) are provided at the top of the reactor body (4), and the feed ports (1) are arranged on the left and right sides of the mounting groove and communicate with the annular reaction chamber.

7. A double-temperature-controlled reactor according to claim 4, characterized in that, A discharge port (8) is provided at the bottom of the reactor body (4), the discharge port (8) is communicated with a discharge pipe, and a filter screen is provided at the port of the discharge pipe.

8. A double-temperature-controlled reactor according to claim 7, characterized in that, The discharge pipe is communicated with a discharge screw pump.

9. A double-temperature-controlled reactor according to claim 4, wherein, Further comprising a universal reactor support (6), and the reactor body (4) is disposed on the universal reactor support (6).

10. A preparation method of an ultra-high viscosity polymer binder, characterized in that, Applying the double-temperature-controlled reactor according to any one of claims 4-9, comprising the following steps: S1: Mixing carboxyl-terminated nitrile rubber, N-(3-aminopropyl)methacrylamide, acrylonitrile, a catalyst and a nonionic surfactant evenly in water, and reacting to prepare a seed emulsion, with a reaction time of 2-4 h and a reaction temperature of 40-60 °C; S2: Adding an alkali solution to methacrylic acid to obtain a methacrylate solution; S3: Add the methacrylate solution and the non-polar monomer to the seed emulsion in sequence. After stirring evenly, an emulsion for reaction is obtained. S4: Under an inert gas atmosphere, drop the initiator into the emulsion for reaction. The reaction time is 8 - 12 h, and the reaction temperature is 40 - 90 °C. After cooling, carry out degassing of monomers, dilution with water, and filtration in sequence to obtain an ultra-high viscosity polymer binder.

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