High-shear dispersion instrument suitable for phase inversion emulsification method

Abstract

The high-shear dispersion instrument comprises a reaction kettle and a high-shear dispersion machine, the reaction kettle is located at the lower end of the high-shear dispersion machine, the reaction kettle is placed on the upper surface of a temperature control electric furnace, and the temperature control electric furnace is used for heating and heat preservation of the reaction kettle. The flow of water added in the paste emulsifying and diluting process is adjusted through a water quantity controller, meanwhile, a relatively stable temperature range is provided for the interior of the reaction kettle through mutual cooperation of a temperature control electric furnace and an electronic energy-saving temperature control instrument, and the paste in the reaction kettle during phase inversion is sheared through a dispersion disc arranged at the lower end of a high-shear dispersion machine, so that the paste in the reaction kettle is emulsified and diluted. Meanwhile, the frame type stirring paddle additionally arranged at the lower end of the high-shear dispersion machine is used for stirring after the paste in the reaction kettle is converted into emulsion, the dispersion disc is combined with the frame type stirring paddle, the high-speed shearing function and the low-speed stirring function are integrated, meanwhile, the temperature control and water control functions are achieved, and operation and use are easy and convenient.

Description

Technical Field

[0001] The utility model relates to the technical field of experimental instruments, in particular to a high shear dispersion instrument suitable for a phase inversion emulsification method. Background Art

[0002] Acrylonitrile-butadiene-styrene (ABS) resin offers excellent mechanical, thermal, electrical, and chemical properties, and its relatively low cost makes it increasingly widely used in electronics, automotive, 3D printing, and other fields. However, the presence of an unsaturated polybutadiene rubber phase in ABS resin makes it susceptible to oxidative degradation under conditions such as light, heat, and oxygen. This is manifested microscopically as polymer chain breakage and macroscopically as yellowing and brittleness, leading to a sharp decline in the material's usability. Adding antioxidant additives to ABS resin can effectively slow oxidative degradation and extend the material's service life. Adding antioxidants to ABS resin in the form of solid powders can cause localized accumulation of the antioxidant within the material, reducing its effectiveness. Preparing a solid powdered antioxidant into an aqueous antioxidant emulsion allows for rapid and uniform dispersion in the ABS graft emulsion, reducing the amount of antioxidant used and improving its effectiveness.

[0003] Currently, most methods for preparing aqueous antioxidant emulsions use a direct emulsification process. First, one or more antioxidants are melted to form an antioxidant eutectic. The eutectic is then cooled to a certain temperature, and then an emulsifier aqueous solution is added. High-speed shearing is applied to maximize the uniformity of the dispersion. Finally, the emulsion is cooled to room temperature while stirring at a low speed to obtain the aqueous antioxidant emulsion. Pilot equipment used in conjunction with these processes includes homogenizers, ultrasonic wave machines, and high-shear machines. Although the emulsion preparation process is simple, the particle size can only reach the micron level. Furthermore, the large amount of external energy required results in poor stability in micron-sized emulsions, preventing them from maximizing the antioxidant efficacy of the antioxidant.

[0004] Phase inversion emulsification involves preparing a eutectic, cooling it to near the phase inversion temperature, then adding an emulsifier and a certain amount of water. Stirring for a certain period of time results in a W / O emulsion. Water is then continuously added to the W / O emulsion, causing phase inversion to transform it into an O / W emulsion, ultimately producing an aqueous emulsion. Antioxidant emulsions prepared using phase inversion emulsification can achieve nanometer-scale particle size. Nanoparticles have a larger specific surface area, allowing the antioxidant to be more evenly distributed within the matrix, thereby maximizing its antioxidant efficacy.

[0005] However, there is currently no small-scale test device suitable for preparing water-based antioxidant emulsions using the phase inversion method. Most of the small-scale experimental devices currently used in the literature are high-speed dispersers or electronic constant-speed stirrers. Among them, high-speed dispersers are only suitable for the early stage of antioxidant phase inversion and when the viscosity of the antioxidant paste is particularly high during the phase inversion. The high shear speed is conducive to the shear dispersion of the paste, but it is not suitable for the later stage when the antioxidant paste is transformed into an antioxidant emulsion. In addition, the high shear force of the high-speed disperser will destroy the emulsion structure, causing the emulsion to break, affecting the stability of the antioxidant emulsion. The electronic constant-speed stirrer is not powerful enough and can reach a speed that is not fast enough. It can neither provide sufficient external energy during the phase inversion of the antioxidant emulsion nor effectively disperse the antioxidant paste in a high-viscosity state, making it difficult to control the particle size of the antioxidant emulsion at the nanometer level. Utility Model Content

[0006] The purpose of the utility model is to provide a high shear dispersion instrument suitable for phase inversion emulsification method, which integrates temperature control, water control, high-speed dispersion and low-speed stirring, and is particularly suitable for preparing nano-emulsions by phase inversion method.

[0007] To achieve the above-mentioned purpose, the present invention provides the following technical solutions: a high-shear dispersion instrument suitable for phase inversion emulsification method, comprising a reactor and a high-shear disperser, the high-shear disperser being fixed by a vertical rod, the reactor being located at the lower end of the high-shear disperser, and a temperature-controlled electric furnace being provided at the lower end of the reactor, the reactor being placed on the upper surface of the temperature-controlled electric furnace, the reactor being heated and insulated by the temperature-controlled electric furnace, and the interior of the reactor being sheared by a dispersion disk provided at the lower end of the high-shear disperser, and the interior of the reactor being stirred by a frame-type stirring paddle provided at the lower end of the high-shear disperser, and the dispersion disk and the frame-type stirring paddle being combined to realize the integration of high-speed shearing and low-speed stirring functions.

[0008] Preferably, the high shear disperser includes a control cabinet, a main machine, a lifting rod and a working head. The lifting rod is clamped and fixed by the upper end of the vertical rod. The main machine slides on the lifting rod, and the working head is located at the lower end of the main machine. The control cabinet is located at the upper end of the lifting rod. The rotation of the main machine and the lifting and lowering of the main machine on the lifting rod are controlled by the control cabinet.

[0009] Preferably, the lower end of the working head is connected to the dispersion disk and the frame-type stirring paddle respectively through provided joints.

[0010] Preferably, the outer wall surface of the lifting rod is provided with scale markings, thereby realizing the identification of the lifting height of the main machine.

[0011] Preferably, a water volume controller is provided at the upper end of the reactor, and the flow rate of water added during the emulsification and dilution process of the paste is adjusted by the water volume controller, which can control the temperature and prevent uneven dilution of the paste.

[0012] Preferably, the high shear dispersion instrument is further provided with an electronic energy-saving temperature controller, which is inserted into the reactor through a temperature probe to monitor the temperature in the reactor in real time, and the temperature probe is connected to the electronic energy-saving temperature controller through an electric wire.

[0013] Preferably, the temperature-controlled electric furnace and the electronic energy-saving temperature controller cooperate with each other to provide a relatively stable temperature range inside the reactor, effectively control the temperature during the phase inversion process, and ensure a smooth cooling during the emulsification process.

[0014] Preferably, the heating temperature of the temperature-controlled electric furnace is adjusted by a knob provided on one side of the temperature-controlled electric furnace.

[0015] Compared with the prior art, the present invention has the following beneficial effects:

[0016] 1. This utility model integrates high-speed shearing and low-speed stirring functions into one, and has the functions of temperature control and water control. It is simple and convenient to operate and use. It is in line with the actual conditions of each stage of the entire phase inversion emulsification process and has a feasible guiding role in accurately controlling the actual working conditions in the phase inversion emulsification method.

[0017] 2. This utility model is fully adapted for emulsification using the phase inversion method. The device is equipped with a dispersing disc and a frame-type stirring paddle. The dispersing disc can be used for high-speed dispersion during phase inversion, and the frame-type stirring paddle can be used for low-speed dispersion and mixing after phase inversion. This utility model solves both the problem of high viscosity and difficulty in dispersing the paste during phase inversion, as well as the problem of difficulty in diluting the paste after phase inversion and the problem of emulsion instability caused by high shear.

[0018] 3. The utility model is equipped with an electronic energy-saving temperature controller and a temperature-controlled electric furnace, which can provide a relatively stable temperature range, effectively control the temperature during the phase inversion process, and ensure a smooth cooling during the emulsification process.

[0019] 4. The utility model is equipped with a water regulator, which can adjust the flow rate of water added during the emulsification and dilution process of the paste, thereby controlling the temperature and preventing uneven dilution of the paste. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention and do not constitute a limitation to the present invention.

[0021] In the attached figure:

[0022] Figure 1 This is a schematic structural diagram of a high shear dispersion instrument suitable for a phase inversion emulsification method according to the present invention;

[0023] Numbers in the figure: 1. Temperature-controlled electric furnace; 101. Knob; 2. Electronic energy-saving temperature controller; 201. Temperature probe; 202. Electric wire; 3. High shear disperser; 301. Control cabinet; 302. Main unit; 303. Lifting rod; 304. Working head; 305. Scale mark; 4. Water volume controller; 501. Dispersion plate; 502. Frame-type stirring paddle; 503. Connector; 6. Reactor. DETAILED DESCRIPTION

[0024] The preferred embodiments of the present invention are described below in conjunction with the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention and are not used to limit the present invention.

[0025] Example: Figure 1 As shown, a high shear dispersion instrument suitable for phase inversion emulsification method includes a reactor 6 and a high shear disperser 3, the high shear disperser 3 is fixed by a vertical rod, the high shear disperser 3 includes a control cabinet 301, a main unit 302, a lifting rod 303 and a working head 304, the lifting rod 303 is clamped and fixed by the upper end of the vertical rod, the main unit 302 is slidably located on the lifting rod 303, and the working head 304 is located at the lower end of the main unit 302, the lower end of the working head 304 is respectively connected to the dispersion disk and the frame-type stirring paddle 502 through a provided joint 503, the control cabinet 301 is located at the upper end of the lifting rod 303, and the rotation of the main unit 302 and the lifting and lowering of the main unit 302 on the lifting rod 303 are respectively controlled by the control cabinet 301, and the outer wall surface of the lifting rod 303 is provided with a scale mark Identification 305 is used to identify the lifting height of the main machine 302. The reactor 6 is located at the lower end of the high shear disperser 3, and a temperature-controlled electric furnace 1 is provided at the lower end of the reactor 6. The reactor 6 is placed on the upper surface of the temperature-controlled electric furnace 1. The heating temperature of the temperature-controlled electric furnace 1 is adjusted by the knob 101 provided on one side of the temperature-controlled electric furnace 1. The reactor 6 is heated and kept warm by the temperature-controlled electric furnace 1. The dispersion disk 501 provided at the lower end of the high shear disperser 3 is used to shear the early phase transition inside the reactor 6 and the state where the viscosity of the paste is particularly large during the phase transition. At the same time, the frame-type stirring paddle 502 provided at the lower end of the high shear disperser 3 is used to stir the paste inside the reactor 6 after it is converted into an emulsion state. The dispersion disk 501 is combined with the frame-type stirring paddle 502 to realize the integration of high-speed shearing and low-speed stirring functions.

[0026] A water volume controller 4 is provided at the upper end of the reaction kettle 6 , and the water volume controller 4 is used to adjust the flow rate of water added during the emulsification and dilution process of the paste, thereby controlling the temperature and preventing uneven dilution of the paste.

[0027] Among them, the high shear dispersion instrument is also provided with an electronic energy-saving temperature controller 2, which is inserted into the reactor 6 through a temperature probe 201 to monitor the temperature in the reactor 6 in real time, and the temperature probe 201 is connected to the electronic energy-saving temperature controller 2 through an electric wire 202. The temperature-controlled electric furnace 1 and the electronic energy-saving temperature controller 2 cooperate with each other to provide a relatively stable temperature range for the inside of the reactor 6, effectively control the temperature during the phase inversion process, and ensure smooth cooling of the emulsification process.

[0028] Taking the preparation of antioxidant emulsion as an example, the specific steps for using the above high shear dispersion instrument are as follows:

[0029] 1) Add 60 g of antioxidant CPL and 40 g of antioxidant DLTDP into a reaction kettle 6, set the temperature of the temperature-controlled electric furnace 1 to about 100° C., use a frame-type stirring paddle 502, and stir at a speed of 200 rpm to form an antioxidant eutectic under these conditions;

[0030] 2) Cooling the antioxidant eutectic to 45° C., the hydrophilic-lipophilic equilibrium temperature of the preformed water-in-oil emulsion, adding the composite emulsifier aqueous solution, and continuing shear mixing for 30 minutes using a dispersion disk 501 at a high speed of 2000 rpm to form a water-in-oil emulsion;

[0031] 3) Using a water controller 4, 70 g of deionized water is slowly added to the water-in-oil emulsion at a constant rate. The temperature is maintained using a temperature-controlled electric furnace 1. A frame-type stirring paddle 502 is used to maintain a moderate speed. Stirring is continued for 10 minutes to cause the water-in-oil emulsion to undergo a phase inversion, becoming an oil-in-water antioxidant emulsion.

[0032] 4) Adding an aqueous solution of an auxiliary agent to the obtained oil-in-water antioxidant emulsion system, maintaining the temperature and stirring rate, continuing stirring for 10 minutes, and then cooling to room temperature under stirring at 150 rpm to obtain an aqueous antioxidant emulsion.

[0033] Finally, it should be noted that the above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art will be able to modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein with equivalents. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. A high shear dispersion apparatus suitable for phase inversion emulsification, characterized by: The invention comprises a reactor and a high shear disperser, wherein the high shear disperser is fixed by a vertical rod, the reactor is located at the lower end of the high shear disperser, and a temperature-controlled electric furnace is provided at the lower end of the reactor. The reactor is placed on the upper surface of the temperature-controlled electric furnace, and the reactor is heated and kept warm by the temperature-controlled electric furnace, and the interior of the reactor is sheared by a dispersion disk provided at the lower end of the high shear disperser, and the interior of the reactor is stirred by a frame-type stirring paddle provided at the lower end of the high shear disperser. By combining the dispersion disk and the frame-type stirring paddle, high-speed shearing and low-speed stirring functions are integrated into one.

2. A high shear dispersion instrument suitable for phase inversion emulsification method according to claim 1, characterized in that: The high shear disperser includes a control cabinet, a main machine, a lifting rod and a working head. The lifting rod is clamped and fixed by the upper end of the vertical rod. The main machine slides on the lifting rod, and the working head is located at the lower end of the main machine. The control cabinet is located at the upper end of the lifting rod. The rotation of the main machine and the lifting and lowering of the main machine on the lifting rod are controlled by the control cabinet.

3. A high shear dispersion instrument suitable for phase inversion emulsification method according to claim 2, characterized in that: The lower end of the working head is connected to the dispersion disk and the frame-type stirring paddle respectively through provided joints.

4. A high shear dispersion instrument suitable for phase inversion emulsification method according to claim 2, characterized in that: The outer wall surface of the lifting rod is provided with scale marks, thereby realizing the identification of the lifting height of the main machine.

5. A high shear dispersion instrument suitable for phase inversion emulsification method according to claim 1, characterized in that: A water volume controller is provided at the upper end of the reactor, and the flow rate of water addition is adjusted by the water volume controller.

6. A high shear dispersion instrument suitable for phase inversion emulsification method according to claim 1, characterized in that: The high shear dispersion instrument is further provided with an electronic energy-saving temperature controller, which is inserted into the reactor through a temperature probe to monitor the temperature in the reactor in real time, and the temperature probe is connected to the electronic energy-saving temperature controller via an electric wire.

7. A high shear dispersion apparatus suitable for phase inversion emulsification according to claim 6, characterized in that: The temperature-controlled electric furnace cooperates with the electronic energy-saving temperature controller to provide a stable temperature range inside the reactor, control the temperature during the phase inversion process, and ensure a smooth temperature drop during the emulsification process.

8. A high shear dispersion apparatus suitable for phase inversion emulsification according to claim 7, characterized in that: The heating temperature of the temperature-controlled electric furnace is adjusted by a knob provided on one side of the temperature-controlled electric furnace.

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