Multi-module impact-coalescence reactor and use method thereof

文档序号:707221 发布日期:2021-04-16 浏览:7次 中文

阅读说明:本技术 一种多模块撞击-聚并反应器及其使用方法 (Multi-module impact-coalescence reactor and use method thereof ) 是由 刘志伟 刘有智 郭豫晋 袁志国 张栋铭 申红艳 张超 于 2020-12-04 设计创作,主要内容包括:本发明公开一种多模块撞击-聚并反应器及其使用方法,该反应器包括细乳化模块、撞击-聚并模块、后处理模块与连接件;所述细乳化模块的上、下对称进液口与进液管路连接,冲洗孔用于洗涤模块,其内部的十字形通道则用于强化细乳液的形成;所述撞击-聚并模块与细乳化模块相连,其外侧设有可视窗,其内部为混合腔,通过流体高速对撞强化液滴间的聚并过程,促进液滴内的化学反应;所述后处理模块与撞击-聚并模块连接,内部空腔安装盘管,用于控制反应温度和停留时间;所述连接件包括A、B和C三种,起到连接各模块以及密封流体的作用。本发明结构简单、组装方便,可解决无机、有机、有机-无机纳米复合材料传统制备过程不连续、可控性差等缺陷。(The invention discloses a multi-module impact-coalescence reactor and a using method thereof, wherein the reactor comprises a fine emulsification module, an impact-coalescence module, a post-treatment module and a connecting piece; the upper symmetrical liquid inlet and the lower symmetrical liquid inlet of the fine emulsification module are connected with a liquid inlet pipeline, the flushing hole is used for washing the module, and the cross-shaped channel in the fine emulsification module is used for strengthening the formation of fine emulsion; the collision-coalescence module is connected with the fine emulsification module, a visual window is arranged on the outer side of the collision-coalescence module, a mixing cavity is arranged in the collision-coalescence module, and the coalescence process among liquid drops is enhanced through high-speed collision of fluid so as to promote chemical reaction in the liquid drops; the post-treatment module is connected with the impact-coalescence module, and a coil is arranged in an internal cavity and used for controlling the reaction temperature and the retention time; the connections include A, B and C, which serve to connect the modules and seal the fluid. The invention has simple structure and convenient assembly, and can overcome the defects of discontinuity, poor controllability and the like of the traditional preparation process of inorganic, organic and organic-inorganic nano composite materials.)

1. A multi-module impact-coalescence reactor, characterized by: the reactor comprises a fine emulsification module, an impact-coalescence module, a post-treatment module and a connecting piece; the upper symmetrical liquid inlet and the lower symmetrical liquid inlet of the fine emulsification module are connected with a liquid inlet pipeline, the flushing hole is used for washing the module, and the cross-shaped channel in the fine emulsification module is used for strengthening the formation of fine emulsion; the impact-coalescence module is connected with the fine emulsification module, a visual window is arranged on the outer side of the impact-coalescence module and used for observing a flow field, a mixing cavity is arranged in the impact-coalescence module, and the coalescence process among liquid drops is strengthened through fluid impact so as to promote the chemical reaction in the liquid drops to be carried out; the post-processing module is connected with the impact-coalescence module, and a coil pipe is arranged in the cavity; the length and the installation form of the built-in coil pipe are adjusted according to actual requirements, and the post-processing module is used for controlling the reaction temperature and the residence time; the connector serves to connect the modules and to seal the fluid.

2. The multi-module impact-coalescence reactor according to claim 1, characterized in that: the fine emulsification module is of a cubic structure, and the upper end surface and the lower end surface of the fine emulsification module are provided with coaxially symmetrical liquid inlets which are connected with a liquid inlet pipe through a joint; the flushing hole on the left side is used for cleaning the interior of the module, and the liquid discharging hole on the right side is connected with the impact-coalescence module through a connecting piece A; the middle parts of the two liquid inlets are provided with through holes, the through holes are connected to form a cross-shaped channel, and fluid is impacted and mixed in the cross-shaped channel to form miniemulsion.

3. The multi-module impact-coalescence reactor according to claim 2, characterized in that: the pore passage on the fine emulsification module adopts national standard M6-M8 type internal threads, and the length of the threads is 10.0-15.0 mm; the inner diameters of the upper and lower symmetrical holes of the cross-shaped through hole are 0.8-1.2 mm, and the lengths are 5.0-10.0 mm; the inner diameter of the through hole on the left side and the right side in the cross-shaped through hole is 1.6-2.4 mm, and the length is 6.0-12.0 mm.

4. The multi-module impact-coalescence reactor according to claim 1, characterized in that: the collision-coalescence module is of a hollow cubic structure, and visible windows are arranged on the front end face, the rear end face and the upper end face of the collision-coalescence module and are used for observing and collecting fluid flow information; the left end face and the right end face of the impact-coalescence module are respectively provided with a coaxial symmetrical liquid inlet which is connected with the fine emulsification module through a connecting piece A, and a through hole in the middle of the liquid inlet is communicated with the cavity; the lower end surface of the impact-coalescence module is provided with a liquid discharge hole, and two streams of fluid respectively flow into the liquid inlets at the left side and the right side and then collide at high speed to form impact flow so as to strengthen the coalescence process of liquid drops and flow out through the liquid discharge hole; and the lower side liquid discharge hole of the impact-coalescence module is connected with the post-treatment module through a B connecting piece.

5. The multi-module impact-coalescence reactor according to claim 4, characterized in that: threaded holes are distributed around the visual window and used for fixing the light-transmitting plate; the specification of the threaded holes around the visual window is M2-M3; the liquid inlet of the impact-coalescence module is provided with M6-M8 type internal threads, and the length of the threads is 10.0-15.0 mm; M8-M10 type internal threads are arranged in a liquid discharge hole of the impact-coalescence module, and the length of the threads is 10.0-15.0 mm; the impact flow rate is 5.0-8.0 m/s.

6. The multi-module impact-coalescence reactor according to claim 1, characterized in that: the post-processing module is of a hollow cubic structure, and a liquid inlet on the upper end surface of the post-processing module is connected with the impact-coalescence module through a connector B; the liquid discharge hole at the lower side of the lower module is connected with the next module; the circulating water interfaces on the left side and the right side are respectively connected with the C connecting piece and used for controlling the post-treatment temperature; the front end face and the rear end face of the post-processing module are provided with visual windows for installing and disassembling an internal pipeline and monitoring the reaction process; the coil pipe is arranged in the cavity of the post-treatment module, the inlet end of the coil pipe is communicated with the connecting piece B, the outlet end of the coil pipe is connected with the liquid discharge hole of the post-treatment module, and the reaction residence time is adjusted by controlling the length of the coil pipe.

7. The multi-module impact-coalescence reactor according to claim 6, characterized in that: threaded holes are distributed around the visual window and used for fixing the light-transmitting plate; the thickness of the shell of the post-processing module is 5.0-8.0 mm, and the specification of threaded holes on the periphery of the visual window is M2-M3; the threads of other channels are national standard M8-M10 type internal threads, and the length of the threads is 5.0-10.0 mm;

the coil pipe is made of any one of silica gel, polyurethane or polytetrafluoroethylene, and is arranged in the post-treatment module in an O-shaped, S-shaped or U-shaped mode, the inner diameter of the pipe is 3.0-5.0 mm, and the wall thickness is 0.2-0.5 mm;

the liquid discharge hole is connected with the outlet end of the coil pipe or connected with another post-treatment module to form a multi-stage post-treatment group for prolonging the reaction retention time.

8. The multi-module impact-coalescence reactor according to claim 1, characterized in that: the connecting piece has three structures of A, B and C:

the fine emulsification module and the impact-coalescence module are connected through a connecting piece A, the connecting piece A is of a cylindrical structure with a through hole in the center, external threads are arranged at two ends of the through hole, and a hexagonal prism is arranged in the middle of the cylinder;

the impact-coalescence module is connected with the post-processing module through a connecting piece B; the connecting piece B is of a cylindrical structure with a plurality of sections of through holes with different inner diameters in the center, a hexagonal prism is arranged in the middle of the cylinder, and a liquid injection hole is formed in the middle of the hexagonal prism and used for adding an initiator or other additives; one end of the hexagonal prism is a straight hole, the other end of the hexagonal prism is a step hole, the length of the step hole is greater than that of the straight hole, and the step hole is used for connecting a coil pipe in the post-processing module;

the aftertreatment module passes through C connecting piece and links to each other with circulating water system, and the C connecting piece is equipped with the cylinder structure of through-hole for the center, and its outside one end is the back taper interface for connect the circulating water hose, and the other end is equipped with M8~ M10 type external screw thread, and the cylindrical middle part is equipped with the hexagonal prism.

9. The multi-module impact-coalescence reactor of claim 8, wherein: the outer diameter of the connecting piece A is 6.0-8.0 mm, and the inner diameter is 1.6-2.4 mm; the outer diameter of the connecting piece B is 8.0-10.0 mm, the inner diameter of the connecting piece B is 6.0-8.0 mm and 4.0-6.0 mm respectively, and the inner diameter of the liquid injection hole is 0.5-1.0 mm; the inner diameter of the C connecting piece is 6.0-8.0 mm, the height of the inverted cone is 5.0-10.0 mm, and the cone angle is 10-30 degrees.

10. A method of using a multi-module impact-coalescence reactor according to any one of claims 1 to 9, characterized by the steps of:

(1) assembling and debugging the reactor: firstly, selecting two groups of fine emulsification modules, connecting a liquid inlet pipe to a liquid inlet, sealing a flushing hole by using a plug, and then installing the fine emulsification modules on two sides of an impact-coalescence module by using an A connecting piece; secondly, the impact-coalescence module is connected with the post-processing module through a connecting piece B, and the light-transmitting plate is fixed outside the visible window by adopting bolts; finally, connecting the coil pipe to the connecting piece B, introducing circulating water into the post-treatment module through the connecting piece C, and fixing a light-transmitting plate outside the visible window by adopting bolts to complete the assembly of the reactor; detecting whether liquid leakage exists or not, sealing conditions and the like, and controlling operation parameters and reaction conditions to finish debugging of the reactor;

(2) operation of the reactor: respectively inputting the equal-volume flow of two strands of oil-water system coarse emulsion with different compositions into the fine emulsification modules at two sides, and forming fine emulsion under the strengthening effect of an impact flow field; the two strands of miniemulsion are respectively introduced into an impact-coalescence module through a connecting piece A, and two strands of fluid impact at a high speed in a mixing zone to initiate the miniemulsion drops to quickly coalesce, so that the nucleation reaction in the drops is promoted; and (3) the polymerized miniemulsion enters a post-treatment module through a connector B, a monomer is subjected to polymerization reaction in a pipeline of the post-treatment module under the conditions of 0-60 ℃ and the action of an initiator, and a product is obtained after 2-10 min.

Technical Field

The invention relates to a multi-module impact-coalescence reactor and a using method thereof, belonging to the fields of chemical reaction engineering, multiphase flow and organic-inorganic nano composite materials.

Background

The organic-inorganic nano composite material taking the polymer as the continuous phase can overcome the defects of poor dispersity, easy agglomeration, difficult processing and the like of single inorganic particles, and can improve the performances of stability, strength and the like of organic macromolecules, so the organic-inorganic nano composite material has wide application prospect in the fields of mechanics, optics, electronics, biology and the like. Common methods for preparing organic-inorganic nanocomposite materials include sol-gel methods, in-situ methods, intercalation methods, self-assembly, and the like. Among them, the in-situ method can be classified into an in-situ polymerization method and an in-situ generation method. The in-situ polymerization method is to uniformly disperse the inorganic nanoparticles with Surface treatment in the monomer solution and then initiate the polymerization of the monomer, and has the advantages of simple operation, uniform dispersion of the inorganic particles in the composite and stable performance of each phase, but the preparation of the inorganic nanoparticles is accompanied by serious agglomeration (J. Li, et al, Applied Surface Science, 2010, 256: 4339-. The inorganic particles adopted by the in-situ generation method are not prepared in advance, but generated in situ in the reaction process, so that the problems can be alleviated, but the dispersion process of the inorganic particles in an organic phase is difficult to control, and the loading capacity is low. In recent years, with the rapid development of miniemulsion technology, a new idea is provided for the preparation of organic-inorganic nanocomposite materials. The miniemulsion polymerization method utilizes a unique mode of 'droplet nucleation' to improve the dispersibility and the loading capacity of inorganic nanoparticles in an organic polymer, can realize nano monodispersion, polymerization growth regulation and uniform dispersion packaging, and is an effective way for preparing organic-inorganic nano composite materials (segmented orchid, and the like, bonding 2017, 38: 47-51; tall party pigeon, and the like, chemical development 2016, 28: 1076, 1083). Tiarks and Winkelmann et al (Tiarks F, et al chem. Phys., 2001, 202: 51-60; Winkelmann M, et al chem. Eng. Sci., 2013, 92: 126-133) improve the traditional miniemulsion polymerization process, and provide a 'miniemulsion coalescence method', which utilizes the continuous rupture-coalescence action of miniemulsion droplets, further realizes the control of reaction and improves the encapsulation rate of inorganic particles; fukui et al (Fukui Y, Fujimoto K.J. Mater. chem., 2012, 22: 3493-3499.) teach that the droplet coalescence method also enables the control of the nucleation and growth processes of the crystals. In addition, the microscopic interface of the fine emulsion liquid drop replaces the millimeter-centimeter grade macroscopic interface of the traditional reactor, so that the mass transfer interface area can be multiplied or even dozens of times, and the mass transfer and reaction rate can be greatly improved (Zhangzhang, chemical reports, 2018, 69: 44-49).

In conclusion, the key technology of miniemulsion polymerization and coalescence is the control technology of miniemulsion system formation and droplet coalescence, but in practice, the formation of miniemulsion and the generation of inorganic particles and polymers are often completed step by step and intermittently (ZL 201610960843.5; ZL201010508507.X; CN201810315123.2; CN 200810079596.3), which results in weak association, poor controllability and low production efficiency of the compounding process. Therefore, there is an urgent need to develop a novel reactor that can continuously and controllably produce an organic-inorganic nanocomposite.

Disclosure of Invention

The invention aims to provide a multi-module impact-coalescence reactor and a using method thereof, which construct a novel reactor integrating processes of fine emulsification, reaction nucleation, monomer polymerization and the like by using a modularized design concept as reference, and solve the problems of poor controllability, incapability of continuous generation and the like of inorganic, organic and organic-inorganic nano composite material preparation processes. The technical scheme adopted by the invention is as follows:

the invention provides a multi-module impact-coalescence reactor, which comprises a fine emulsification module, an impact-coalescence module, a post-treatment module and a connecting piece.

The fine emulsification module is of a cubic structure, and the upper end surface and the lower end surface of the fine emulsification module are provided with coaxially symmetrical liquid inlets which are connected with a liquid inlet pipe through a joint; the flushing hole on the left side is used for cleaning the interior of the module, and the liquid discharging hole on the right side is connected with the impact-coalescence module through a connecting piece A; the middle parts of the two liquid inlets are provided with through holes, the through holes are connected to form a cross-shaped channel, and fluid is impacted and mixed in the cross-shaped channel to form miniemulsion; the pore passage on the fine emulsification module adopts national standard M6-M8 type internal threads, and the length of the threads is 10.0-15.0 mm; the inner diameters of the upper and lower symmetrical through holes of the cross-shaped channel are both 0.8-1.2 mm, and the lengths are both 5.0-10.0 mm; the inner diameter of the through hole on the left side and the right side in the cross-shaped channel is 1.6-2.4 mm, and the length is 6.0-12.0 mm.

The collision-coalescence module is of a hollow cubic structure, and visible windows are arranged on the front end face, the rear end face and the upper end face of the collision-coalescence module and are used for observing and collecting fluid flow information; threaded holes are distributed around the visual window and used for fixing the light transmission plate; the left end face and the right end face of the impact-coalescence module are respectively provided with a coaxial symmetrical liquid inlet which is connected with the fine emulsification module through a connecting piece A, and a through hole in the middle of the liquid inlet is communicated with the cavity; the lower end surface of the impact-coalescence module is provided with a liquid discharge hole, and two streams of fluid respectively flow into the liquid inlets at the left side and the right side and then collide at high speed to form impact flow so as to strengthen the coalescence process of liquid drops and flow out through the liquid discharge hole; the lower side liquid discharge hole of the impact-coalescence module is connected with the post-processing module through a connecting piece B; the specification of the internal thread holes on the periphery of the visual window is M2-M3; the liquid inlet of the impact-coalescence module is provided with M6-M8 type internal threads, and the length of the threads is 10.0-15.0 mm; M8-M10 type internal threads are arranged in a liquid discharge hole of the impact-coalescence module, and the length of the threads is 10.0-15.0 mm; the impact flow rate is 5.0-8.0 m/s.

The post-processing module is of a hollow cubic structure, and a liquid inlet on the upper end surface of the post-processing module is connected with the impact-coalescence module through a connector B; the liquid discharge hole at the lower side of the device can be communicated with the connecting piece B or connected with another post-treatment module to form a multi-stage post-treatment group for prolonging the reaction retention time; the circulating water interfaces on the left side and the right side are respectively connected with the C connecting piece and used for controlling the post-treatment temperature; the front end face and the rear end face of the post-processing module are provided with visual windows for installing and disassembling an internal pipeline and monitoring the reaction process; threaded holes are distributed around the visual window and used for fixing the light transmission plate; the coil is arranged in the cavity of the post-treatment module and is arranged in the cavity of the post-treatment module in different coiling modes, the inlet of the coil is communicated with the connecting piece B, the outlet end of the coil is connected with the liquid discharge hole of the post-treatment module, and the reaction residence time can be adjusted by controlling the length of the coil; the thickness of the shell of the post-processing module is 5.0-8.0 mm, and the specification of threaded holes on the periphery of the visual window is M2-M3; other pore channels are national standard M8-M10 type internal threads, and the length of the threads is 5.0-10.0 mm; the built-in pipeline can be made of any one of silica gel, polyurethane or polytetrafluoroethylene, can be coiled in various modes such as O-shaped, S-shaped and U-shaped modes and is installed in the post-processing module, the inner diameter of the pipeline is 3.0-5.0 mm, and the wall thickness is 0.2-0.5 mm.

The connecting piece has A, B and C structures: the connecting piece A is of a cylindrical structure with a through hole in the center, external threads are arranged at two ends of the through hole, and a hexagonal prism is arranged in the middle of the cylinder; the connecting piece B is of a cylindrical structure with a plurality of sections of through holes with different inner diameters in the center, a hexagonal prism is arranged in the middle of the cylinder, and a liquid injection hole is formed in the middle of the hexagonal prism and can be used for adding an initiator or other additives; one end of the hexagonal prism is a straight hole, the other end of the hexagonal prism is a step hole, the length of the step hole is greater than that of the straight hole, and the step hole is used for connecting a coil pipe in the post-processing module; the C connecting piece is the cylinder structure that the center was equipped with the through-hole, and its outside one end is the back taper interface for connect the circulating water hose, and the other end is equipped with M8~ M10 type external screw thread, and the columniform middle part is equipped with the hexagonal prism.

The outer diameter of the connecting piece A is 6.0-8.0 mm, and the inner diameter is 1.6-2.4 mm; the outer diameter of the connecting piece B is 8.0-10.0 mm, the inner diameter of the connecting piece B is 6.0-8.0 mm and 4.0-6.0 mm respectively, and the inner diameter of the liquid injection hole is 0.5-1.0 mm; the inner diameter of the C connecting piece is 6.0-8.0 mm, the height of the inverted cone is 5.0-10.0 mm, and the cone angle is 10-30 degrees.

The invention provides a using method of a multi-module impact-coalescence reactor, which comprises the following steps:

(1) assembling and debugging the reactor: firstly, selecting two groups of fine emulsification modules, connecting a liquid inlet pipe to a liquid inlet, sealing a flushing hole by using a plug, and then installing the fine emulsification modules on two sides of an impact-coalescence module by using an A connecting piece; secondly, the impact-coalescence module is connected with the post-processing module through a connecting piece B, and the light-transmitting plate is fixed outside the visible window by adopting bolts; finally, connecting the coil pipe to the connecting piece B, introducing circulating water into the post-treatment module through the connecting piece C, and fixing a light-transmitting plate outside the visible window by adopting bolts to complete the assembly of the reactor; detecting whether liquid leakage exists or not, sealing conditions and the like, and controlling operation parameters and reaction conditions to finish debugging of the reactor;

(2) operation of the reactor: respectively inputting the equal-volume flow of two strands of oil-water system coarse emulsion with different compositions into the fine emulsification modules at two sides, and forming fine emulsion under the strengthening effect of an impact flow field; the two strands of miniemulsion are respectively introduced into an impact-coalescence module through a connecting piece A, and two strands of fluid impact at a high speed in a mixing zone to initiate the miniemulsion drops to quickly coalesce, so that the nucleation reaction in the drops is promoted; and (3) the polymerized miniemulsion enters a post-treatment module through a connector B, a monomer is subjected to polymerization reaction in a pipeline of the post-treatment module at the temperature of 0-60 ℃ and under the condition of an initiator, and a product is obtained after 2-10 min.

The invention provides a multi-module impact-coalescence reactor which can be applied to the continuous and controllable synthesis of organic, inorganic and organic-inorganic nano composite materials.

The invention has the following beneficial effects:

(1) the invention is based on the modularized design concept, combines the characteristics of a miniemulsion polymerization method, constructs a multi-module impact-polymerization reactor, has simple structure of each component module, is convenient to connect and assemble, is easy to clean and maintain, and can realize the regulation and control of the chemical reaction process and the continuous preparation of nano materials;

(2) because the shearing, collision and cavitation of the fluid are enhanced in the confined space, the cracking and coalescence processes of emulsion droplets are enhanced, the refinement of the droplets is promoted, and the nucleation reaction in the nano droplets is regulated and controlled;

(3) in view of the advantages of cheap and easily-obtained millimeter-scale channels (5.0 mm), large specific surface area, adjustable length and the like, the method can be used for enhancing the heat transfer rate of a medium, promoting the polymerization system to be uniformly heated and easily regulating and controlling the reaction temperature and the retention time;

(4) the invention can be used for preparing various inorganic, organic and organic-inorganic nano composite materials, overcomes the defects of discontinuity, poor controllability and the like of the traditional preparation process, and provides new equipment and technical guidance for the development of new chemical materials.

Drawings

FIG. 1 is a front view (A-A cross-sectional view), a top view and a left side view of a fine emulsification module of the present invention;

FIG. 2 is a front view (B-B half section), top view and left side view of the impact-coalescence module of the present invention;

FIG. 3 is a front view (C-C semi-sectional view), top view and left side view of an aftertreatment module of the invention;

FIG. 4 is a front view (D-D cross-sectional view), top view and left side view of the connector A of the present invention;

FIG. 5 is a front view (E-E cross-sectional view), a top view and a left side view of a connector B of the present invention;

FIG. 6 is a front view (F-F section), top view and left side view of a C connection of the present invention;

FIG. 7 is a schematic view of the assembled multi-module impact-coalescence reactor of the present invention;

FIG. 8 is a simplified process flow diagram for preparing nanomaterials using a multi-module impact-coalescence reactor according to the present invention.

In the figure: 1-fine emulsification module; 2, an upper liquid inlet of the fine emulsification module; 3-a lower liquid inlet of the fine emulsification module; 4-liquid discharge hole of fine emulsification module; 5-flushing holes of a fine emulsification module; 6-a cross-shaped channel; 7-impact-coalescence module; 8-front visual window threaded hole; 9-impact-coalescence module front visible window; 10-impact-coalescence module right liquid inlet; 11-left inlet of impact-coalescence module; 12-circular through hole; 13-impact-coalescence module drain hole; 14-a view port on the impact-coalescence module; 15-upper visual window threaded hole; 16-a post-processing module; 17-liquid inlet of post-treatment module; 18-circulating water upper right interface; 19-circulating water left lower interface; 20-coil pipe; 21-visual window threaded hole; 22 — post-processing module visual window; 23-post-treatment module drain hole; 24-a connector; 25-a through hole of the connector; 26-B connectors; 27-liquid injection hole of the connecting piece B; 28-B connector stepped bore; 29-C connector; 30-inverted cone interface; 31-a stirring tank; 32-a fluid delivery device; 33-a flow meter; 34-a flow divider; 35-laser beam; 36-a multi-module impingement-coalescence reactor; 37-circulating water inlet; 38-circulating water outlet; 39 — a sample collector; 40-sample testing device.

Detailed Description

The present invention is further illustrated by, but is not limited to, the following examples.

First, the structure of the present invention will be described, and as shown in fig. 1 to 8, a multi-module impact-coalescence reactor includes a fine emulsification module 1 (see fig. 1), an impact-coalescence module 7 (see fig. 2), a post-treatment module 16 (see fig. 3), an a connection member 24 (see fig. 4), a B connection member 26 (see fig. 5), and a C connection member 29 (see fig. 6).

The upper and lower both sides of the fine emulsification module 1 are provided with coaxially symmetrical liquid inlets: the upper liquid inlet 2 of the fine emulsification module and the lower liquid inlet 3 of the fine emulsification module are connected with a liquid inlet pipe through a joint; the left fine emulsification module flushing hole 5 is used for cleaning the inside of the module, and the right fine emulsification module liquid discharge hole 4 is connected with the impact-coalescence module 7 through an A connecting piece 24; the middle parts of the two liquid inlets are provided with through holes, the through holes are connected to form a cross-shaped channel 6, and fluid is impacted and mixed in the cross-shaped channel 6 to form miniemulsion; the pore channels (2-5) on the fine emulsification module 1 adopt national standard M6-M8 type internal threads, and the length of the threads is 10.0-15.0 mm; the inner diameters of the upper and lower symmetrical through holes of the cross-shaped channel 6 are both 0.8-1.2 mm, and the lengths are both 5.0-10.0 mm; the inner diameter of the through holes on the left side and the right side in the cross-shaped channel 6 is 1.6-2.4 mm, and the length is 6.0-12.0 mm.

The front side, the rear side and the upper side of the impact-coalescence module 7 are provided with an impact-coalescence module front visual window 9 and an impact-coalescence module upper visual window 14 for observing and collecting fluid flow information; the periphery of the visible window is respectively provided with a front visible window threaded hole 8 and an upper visible window threaded hole 15 which are used for fixing the light-transmitting plate; the left side and the right side of the impact-coalescence module 7 are respectively provided with a right liquid inlet 10 and a left liquid inlet 11 of the impact-coalescence module which are coaxially and symmetrically arranged, the impact-coalescence module is connected with the fine emulsification module 1 through an A connecting piece 24, and a circular through hole 12 in the middle of the right liquid inlet 10 and the left liquid inlet 11 of the impact-coalescence module is communicated with the cavity; after the two streams of fluid respectively flow in from the liquid inlets at the left side and the right side, colliding to form an impinging stream under the condition that the flow speed is 5.0-8.0 m/s, strengthening the liquid drop coalescence process, and flowing out through a liquid discharge hole 13 of an impinging-coalescence module; the lower side of the impact-coalescence module 7 is provided with an impact-coalescence module liquid discharge hole 13 which is connected with the post-treatment module 16 through a B connecting piece 26; the front visual window threaded hole 8 and the upper visual window threaded hole 15 are in the specification of M2-M3; M6-M8 type internal threads are arranged on a right liquid inlet 10 and a left liquid inlet 11 of the impact-coalescence module 7, and the length of the threads is 10.0-15.0 mm; M8-M10 type internal threads are arranged on the liquid discharge hole 13 of the impact-coalescence module, and the length of the threads is 10.0-15.0 mm.

The post-treatment module liquid inlet 17 at the upper side of the post-treatment module 16 is connected with the impact-coalescence module 7 through a B connecting piece 26; the post-treatment module liquid discharge hole 23 on the lower side can be communicated with a B connecting piece 26 or connected with another post-treatment module 16 to form a multi-stage post-treatment group for prolonging the reaction retention time; the circulating water right upper interface 18 and the circulating water left lower interface 19 on the left side and the right side are respectively connected with two C connecting pieces 29 and used for controlling the post-treatment temperature; the front and the rear sides of the post-processing module 16 are provided with post-processing module visual windows 22 for installing and disassembling the internal coil pipe 20 and monitoring the reaction process; visual window threaded holes 21 are distributed around the visual window and used for fixing the light-transmitting plate; the post-treatment module is internally provided with a coil pipe 20, the inlet of the coil pipe is communicated with a B connecting piece 26, the outlet end of the coil pipe is connected with a liquid discharging hole 23 of the post-treatment module, and the reaction residence time can also be adjusted by controlling the length of the coil pipe 20; the thickness of the shell of the post-processing module 16 is 5.0-8.0 mm, and the specification of the visual window threaded hole 21 is M2-M3; the liquid inlet 17 of the post-treatment module, the right upper circulating water interface 18, the left lower circulating water interface 19 and the liquid discharge hole 23 of the post-treatment module are all national standard M8-M10 type internal threads, and the thread length is 5.0-10.0 mm; the built-in coil pipe 20 can be made of any one of silica gel, polyurethane or polytetrafluoroethylene, can be coiled in various modes such as O-shaped, S-shaped and U-shaped modes and is installed in the post-processing module, the inner diameter of the coil pipe is 3.0-5.0 mm, and the wall thickness of the coil pipe is 0.2-0.5 mm.

The connecting piece has A, B and C structures: the two ends of the pipeline of the A connecting piece 24 are provided with external threads, the middle part of the pipeline is provided with a hexagonal prism, and the interior of the pipeline is provided with a through hole 25; a liquid injection hole 27 is formed in the middle of the B connecting piece 26 and used for adding an initiator or other auxiliaries, and a step hole 28 is formed in the longer end and used for connecting the coil pipe 20 in the post-treatment module 16; one end of the C connecting piece 29 is an inverted cone connector 30 used for connecting a circulating water hose, and the other end of the C connecting piece is provided with an M8-M10 type external thread connector; the outer diameter of the A connecting piece 24 is 6.0-8.0 mm, and the inner diameter is 1.6-2.4 mm; the outer diameter of the B connecting piece 26 is 8.0-10.0 mm, the inner diameter is 6.0-8.0 mm and 4.0-6.0 mm respectively, and the inner diameter of the liquid injection hole is 0.5-1.0 mm; the inner diameter of the C connecting piece 29 is 6.0-8.0 mm, the height of the inverted cone is 5-10 mm, and the cone angle is 10-30 degrees.

The following is a description of the method of use of a multi-module impact-coalescence reactor of the present invention, as shown in FIG. 5:

the specific assembling steps are as follows: firstly, selecting two groups of fine emulsification modules 1, connecting a liquid inlet pipe to an upper liquid inlet 2 and a lower liquid inlet 3 of the fine emulsification modules, sealing flushing holes 5 of the fine emulsification modules by using plugs, and then installing the fine emulsification modules 1 on two sides of an impact-coalescence module 7 through an A connecting piece 24; secondly, the impact-coalescence module 7 is connected with the post-processing module 16 through a B connecting piece 26, and light-transmitting plates are fixed outside a visible window 9 in front of the impact-coalescence module and a visible window 14 on the impact-coalescence module by bolts; finally, the two ends of the coil 20 are mounted on the B connecting piece 26, then the circulating water is led into the post-treatment module 16 through the C connecting piece 29, and the light-transmitting plate is fixed outside the visible window 22 of the post-treatment module by adopting bolts, thus completing the assembly of the multi-module impact-coalescence reactor 36; detecting whether liquid leakage exists or not, sealing conditions and the like, and controlling operation parameters and reaction conditions to finish debugging of the reactor;

the specific operation steps are as follows: two oil-water systems with different compositions form coarse emulsion in the stirring tank 31, the equal-volume flow of the two coarse emulsion is respectively input into the fine emulsification modules 1 at two sides, and the fine emulsion is formed under the strengthening effect of an impact flow field; the two strands of miniemulsion are respectively led into an impact-coalescence module 7 through an A connecting piece 24, and are impacted at a high speed in a mixing area to initiate the miniemulsion drops to be coalesced quickly, so that the nucleation reaction in the drops is promoted; the polymerized miniemulsion enters the post-treatment module 16 through a connector B26, monomers are subjected to polymerization reaction in the built-in coil pipe 20 of the post-treatment module 16 at the temperature of 0-60 ℃ and under the condition of an initiator, and a product is obtained after 2-10 min.

The following description of the invention is given by way of specific examples:

example 1: a multi-module impact-coalescence reactor is disclosed for testing the fluid mechanical performance.

In the embodiment, a Particle Image Velocimetry (PIV) method is adopted to obtain the flow field information of the two-phase flow of the multi-module impact-coalescence reactor, so as to provide theoretical guidance for the subsequent preparation and application of the nano material.

The specific testing steps are as follows: deionized water is used as a water-phase working medium, and a small amount of water-soluble trace particles are added; cyclohexane is adopted as an oil phase working medium; after the oil phase and the water phase are stirred and mixed, the two phases are respectively input into a multi-module impact-coalescence reactor 36 from liquid inlets of two fine emulsification modules 1 with the same volume flow, two streams of fluid subjected to fine emulsification treatment are ejected from circular through holes 12 at two sides of an impact-coalescence module 7, and impact coalescence is carried out in a limited space; the merged fluid enters the post-treatment module 16 and is discharged through a post-treatment module liquid discharge hole 23; after the fluid flow is stable, starting a laser controller, and irradiating a mixing area by a laser beam 35 from the upper part of the visible window 14 on the impact-coalescence module; starting a CCD camera, and adjusting the intensity of a laser and a laser plane; and (4) calibrating, focusing and shooting by using the Insight 4G software respectively to finally obtain flow field information such as an instantaneous velocity field, an average velocity field, a turbulent kinetic energy field and the like.

Example 2: preparing the inorganic nano material by using the multi-module impact-coalescence reactor.

In the embodiment, the inorganic nano electrode material is prepared by a multi-module impact-coalescence reactor and combining a fine emulsion coalescence method, and the particle size distribution of inorganic particles are controlled by utilizing the micro-scale space effect of nano liquid drops, so that the electrochemical performance of the inorganic nano electrode material is enhanced. FIG. 6 is a flow chart of the process for preparing inorganic nanomaterials using the multi-module impact-coalescence reactor of this example, in particular manganese dioxide (MnO)2) The preparation process of (A) is described as an example.

The specific operation steps are as follows: respectively preparing 0.1 mol/L KMnO4Solution A and 0.15 mol/L MnSO4Solution B; respectively mixing the solution A and the solution B with cyclohexane in a volume ratio of 1:10 by using Span 80 as an emulsifier to prepare water-in-oil type coarse emulsions C and D, and mixing the two flowsThe bodies are introduced into the multi-module impact-coalescence reactor 36 from both sides, respectively; further forming miniemulsions E and F under the action of a miniemulsion module 1, colliding the two streams of fluid in an impact-coalescence module 7 at a volume flow ratio of 1:1, controlling the reaction temperature to be 60 ℃ and the retention time to be about 10 min after the mixed solution enters a post-treatment module 16; and (3) carrying out vacuum filtration, washing and drying on the product, and then preparing the powder material into a working electrode. Test results show that the specific capacitance of a sample prepared by the reactor is 310F/g, which is improved by 10-15% compared with the traditional preparation process, and the specific capacitance is attenuated by 8-10% after circulation for 2000 times.

Example 3: preparing the organic nano material by using the multi-module impact-coalescence reactor.

In the embodiment, the organic nano electrode material is prepared by a multi-module impact-coalescence reactor and combining a fine emulsion coalescence method, and the growth of the polymer is controlled by utilizing the micro-scale space effect of nano liquid drops, so that the electrochemical performance of the polymer is adjusted. Fig. 6 shows a process flow chart of the preparation of organic nanomaterials by using the multi-module impact-coalescence reactor of this embodiment, and specifically, the preparation process of polypyrrole (PPy) is taken as an example for illustration.

The specific operation steps are as follows: dissolving Py monomer and emulsifier in cyclohexane to form oil phase A, dissolving oily initiator in cyclohexane to form oil phase B, mixing the two oil phases with deionized water at a volume ratio of 1:10 to obtain oil-in-water type coarse emulsions C and D, and introducing the coarse emulsions into a multi-module impact-coalescence reactor 36 from two sides respectively; under the action of the fine emulsification module 1, further forming fine emulsions E and F, carrying out collision coalescence on the two streams of fluid in a collision-coalescence module 7 at a volume flow ratio of 1:1, controlling the reaction temperature to be 0 ℃ and the retention time to be about 10 min after the mixed solution enters a post-treatment module 16; and (3) carrying out vacuum filtration, washing and drying on the product, and then preparing the powder material into a working electrode. Test results show that the specific capacitance of a sample prepared by the reactor is 70F/g, which is improved by 20-30% compared with the traditional preparation process, and the specific capacitance is attenuated by 10-15% after circulation for 2000 times.

Example 4: preparing the organic-inorganic nano composite material by using the multi-module impact-coalescence reactor.

The organic-inorganic composite material has the characteristic superior to that of a single component, and the continuous and controllable preparation of the composite material can be realized by adopting a multi-module impact-coalescence reactor. FIG. 6 shows a flow chart of the process for preparing an organic-inorganic composite material using the multi-module impact-coalescence reactor of this example, specifically manganese dioxide/polypyrrole (MnO)2The preparation of the/PPy) is illustrated by way of example.

The specific operation steps are as follows: preparing 0.1 mol/L KMnO4Solution A and 0.15 mol/L MnSO4Solution B; dissolving a Py monomer and an emulsifier in cyclohexane to form an oil phase C, and dissolving an oily initiator in cyclohexane to form an oil phase D; preparing two groups of crude emulsions A-D and B-C in a stirring tank 31 according to the volume ratio of 1:10 respectively; further obtaining miniemulsions E and F through a miniemulsion module 1, and inputting the two miniemulsions into an impact-coalescence module 7 according to the volume flow ratio of 1: 1; after the mixed fluid enters the post-treatment module 16, the reaction temperature is adjusted to be 25 ℃, the retention time is 10 min, and MnO is obtained2a/PPy nanocomposite. Test results show that the specific capacity of a sample prepared by the reactor is 405F/g, the performance of the sample is improved by 10-15% compared with that of a single material, and after the sample is cycled for 2000 times, the capacity retention rate is 90-95%.

16页详细技术资料下载
上一篇:一种医用注射器针头装配设备
下一篇:一种用于井下天然气的耐高温高压复合型脱硫剂及生产设备

网友询问留言

已有0条留言

还没有人留言评论。精彩留言会获得点赞!

精彩留言,会给你点赞!