A micro-reactor suitable for fast reaction of two liquid phase raw materials to generate solid phase product

Abstract

The application discloses a micro-reactor suitable for fast reaction of two liquid-phase raw materials to generate solid-phase products, and is characterized in that the micro-reactor comprises a reactor body, a first distributor and a second distributor are arranged in the reactor body from top to bottom, the reactor body is divided into three chambers, i.e., an upper chamber, a middle chamber and a lower chamber, a first feeding port is arranged at the top of the reactor body, a first discharging port is arranged at the bottom of the reactor body, a second feeding port is arranged at one side of the side wall of the lowermost chamber, a second discharging port is arranged at the other side of the side wall of the lowermost chamber, the second feeding port is higher than the second discharging port, and the second discharging port is communicated with the middle chamber through a circulating pipeline. The product particles produced by the reactor are small in particle size and narrow in particle size distribution range, so that the process is more stable, and the operation control is simple and easy to implement during industrial use; the product is good in repeatability and stable in quality.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical reactor, in particular to a micro reactor suitable for rapid reaction of two liquid phase raw materials to generate solid phase products. BACKGROUND

[0002] The industrial production of rapid reaction of two liquid phase raw materials to generate solid phase products adopts a large stirring tank, but the mixing time of the large stirring tank is in seconds, and the mixing scale is in millimeters, which is not matched with the rapid reaction; the shear force is small, and the agglomeration of the produced solid product is obvious, the diffusion speed of the material in the agglomerate is slowed down, so that the concentration of the reactant slurry in the reaction kettle is not easy to quickly reach uniform, which easily causes local low supersaturation, thereby making the particle size of the product large and the particle size distribution wide; it is easy to cause unstable process and increase the difficulty of operation control; it is easy to cause large fluctuations in product quality.

[0003] Micro-dispersion technology takes micro-structure elements as the core, and strengthens mixing, dispersion and transmission by reducing the dispersion scale of the system in a micron or sub-millimeter limited space, thereby improving the controllability and efficiency of the process. With the reduction of the dispersion scale, the controllability of the fluid in the micro-structure device is strengthened, and rapid mixing can be achieved within milliseconds, which is matched with the reaction speed, and is helpful to quickly reach uniform concentration of the product slurry. Therefore, the present application provides a micro reactor suitable for rapid reaction of two liquid phase raw materials to generate solid phase products by using micro-dispersion technology. SUMMARY

[0004] The present application aims to provide a micro reactor suitable for rapid reaction of two liquid phase raw materials to generate solid phase products, so as to solve the problem of inaccurate reaction process control and poor process operation controllability in the prior art when a large stirring tank is used for rapid reaction of two liquid phase raw materials to generate solid phase products.

[0005] To achieve the above-mentioned purpose, the present application provides a micro reactor suitable for rapid reaction of two liquid phase raw materials to generate solid phase products, comprising: a reactor body, a first distributor and a second distributor are arranged in the reactor body from top to bottom, so as to divide the reactor body into three chambers, i.e., upper, middle and lower chambers; a first feed inlet is arranged at the top of the reactor body, a first discharge outlet is arranged at the bottom of the reactor body, a second feed inlet is arranged at one side of the side wall of the lowermost chamber, and a second discharge outlet is arranged at the other side of the side wall of the lowermost chamber; the second feed inlet is higher than the second discharge outlet; and the second discharge outlet is communicated with the middle chamber through a circulation pipeline.

[0006] The micro reactor suitable for rapid reaction of two liquid phase raw materials to generate solid phase products, the first feed inlet is connected with a feed pipeline and a flow meter.

[0007] The micro reactor suitable for rapid reaction of two liquid phase raw materials to generate solid phase products, a pump and a flow meter are arranged on the circulation pipeline.

[0008] The microreactor suitable for the fast reaction of two liquid-phase raw materials to generate solid-phase products has a third distributor at the second feeding port, and is externally connected with a feeding pipeline and a flow meter.

[0009] The microreactor suitable for the fast reaction of two liquid-phase raw materials to generate solid-phase products has a straight cylinder type inside the reactor body, and an inner diameter of 5-20 cm.

[0010] The microreactor suitable for the fast reaction of two liquid-phase raw materials to generate solid-phase products has a vertical distance between the second feeding port and the second discharging port of greater than or equal to 5 cm.

[0011] The microreactor suitable for the fast reaction of two liquid-phase raw materials to generate solid-phase products has a disc-shaped hole flow type structure of the distributor.

[0012] The microreactor suitable for the fast reaction of two liquid-phase raw materials to generate solid-phase products has a pore diameter of 10-1500 µm of the holes on the first distributor and the second distributor.

[0013] The microreactor suitable for the fast reaction of two liquid-phase raw materials to generate solid-phase products has a pore diameter of 0.1-1000 µm of the third distributor.

[0014] The microreactor suitable for the fast reaction of two liquid-phase raw materials to generate solid-phase products has a component for enhancing the mixing intensity arranged on the inner wall of the intermediate chamber.

[0015] The microreactor suitable for the fast reaction of two liquid-phase raw materials to generate solid-phase products is sealed and connected between the distributor and the reactor body through a flange.

[0016] The microreactor suitable for the fast reaction of two liquid-phase raw materials to generate solid-phase products has a stainless steel material for the inner wall of the reactor body and the distributor.

[0017] The microreactor suitable for the fast reaction of two liquid-phase raw materials to generate solid-phase products has a stainless steel material for the inner wall of the reactor body and the distributor.

[0018] The microreactor suitable for the fast reaction of two liquid-phase raw materials to generate solid-phase products has a stainless steel material for the inner wall of the reactor body and the distributor.

[0019] The reactor body comprises two distributors and three chambers, wherein the upper and middle chambers are dilution units and the lower chamber is a reaction unit. The reactor is suitable for the process of fast reaction of two liquid phase raw materials to generate solid phase products and is also suitable for industrial product production. The design combines micro-dispersion technology to reduce the size of raw material droplets, disperses one raw material into another raw material in the form of micro-droplet groups, forms a uniformly dispersed mixed form, effectively controls the supersaturation of the system in the micron scale range, thereby controlling the nucleation and growth behavior of particles at the micron level, improving the mass transfer efficiency of the reaction process, and very effectively improving the mass transfer deficiency of large stirred tanks. The product particle size is small, the particle size distribution range is narrow, the process is more stable during industrial use, the operation control is simple and easy to operate, the product properties have good repeatability, and the quality is stable. Therefore, the micro-reactor is suitable for the process of fast reaction of two liquid phase raw materials to generate solid phase products and is also suitable for industrial scale production of products. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 The structure diagram of the micro-reactor for fast reaction of two liquid phase raw materials to generate solid phase products is shown in the figure.

[0021] Figure 2 The comparison chart of the change of key process parameters in the preparation of γ-Al2O3 using the device and the change of key process parameters in the preparation of γ-Al2O3 using the traditional method.

[0022] Among them, the reference signs are:

[0023] 1, 5, 7 flow meter

[0024] 2 first distributor

[0025] 3 second distributor

[0026] 4, 6 pump

[0027] 8 third distributor

[0028] 9 reactor DETAILED DESCRIPTION

[0029] The present application will be described in detail below by examples. It is necessary to point out here that the following examples are only used to further illustrate the present application and cannot be understood as limiting the protection scope of the present application. Those skilled in the art can make some non-essential improvements and adjustments to the present application according to the above content of the present application.

[0030] As Figure 1As shown, the present application is suitable for the micro-reactor for fast reaction of two liquid raw materials to generate solid product, which comprises a reactor body, a first distributor 2 and a second distributor 3 arranged in the reactor body from top to bottom, so as to divide the reactor body into three chambers, i.e. an upper chamber, a middle chamber and a lower chamber. The upper chamber is formed between the top of the reactor body and the first distributor 2, the middle chamber is formed between the first distributor 2 and the second distributor 3, and the lower chamber is formed between the second distributor 3 and the bottom of the reactor body. The upper chamber and the middle chamber are dilution units, and the lower chamber is a reaction unit. The top of the reactor body is provided with a first feeding port for feeding a liquid material into the reactor, and the bottom of the reactor body is provided with a first discharging port for discharging the material after reaction out of the reactor into a reaction kettle 9. The first feeding port is connected with a feeding pipeline and a flow meter 1. A second feeding port is arranged on one side wall of the lower chamber, and the second feeding port is connected with a feeding pipeline, a pump 6 and a flow meter 7. A second discharging port is arranged on the other side wall of the lower chamber. The position of the second feeding port on the side wall is higher than that of the second discharging port. Another reaction liquid enters the lower chamber through the second feeding port and reacts with the material from the first feeding port. The second feeding port is also provided with a membrane structure fitting and a third distributor 8. The second discharging port is communicated with the middle chamber through a circulating pipeline, and the circulating pipeline is provided with a pump 4 and a flow meter 5. The reaction liquid in the lower chamber returns to the middle chamber through the circulating pipeline.

[0031] The upper chamber, the middle chamber and the lower chamber are all straight cylinders with the same inner diameter of 5-20 cm.

[0032] The vertical distance between the second feeding port and the second discharging port is greater than or equal to 5 cm. The ratio of the flow rate of the reflux liquid extracted from the lower chamber to the flow rate of the raw materials entering the lower chamber (including the raw materials entering through the first feeding port and the raw materials entering through the second feeding port) is 5-15.

[0033] The distributor is a circular disc-shaped hole flow structure. The hole diameter of the first distributor and the second distributor is 10-1500 μm. The hole diameter of the third distributor is 0.1-1000 μm. The distributor is sealingly connected with the reactor body through a flange.

[0034] The inner wall of the middle chamber is provided with a component for enhancing the mixing intensity. The inner wall of the reactor body and the distributor are made of stainless steel.

[0035] Example 1

[0036] The micro-reactor device is suitable for fast reaction of two liquid phase raw materials to generate solid phase product. Two disc-shaped hole flow distributors are arranged inside the micro-reactor, and the hole diameter is 1000 μm. The two distributors divide the micro-reactor into three chambers from top to bottom. The two chambers on the top are dilution units, the chamber at the bottom is a reaction unit, the cross sections of the three chambers are circular, and the diameters are all 15 cm. The middle chamber is provided with a component for enhancing mixing intensity. The chambers are sealed and connected by flanges at the positions of the distributors. The top of the upper chamber is provided with a feed inlet, and a feed pipe and a flow meter are connected thereto. The side wall of the middle chamber is provided with a feed inlet, and a reflux pipe and a flow meter are connected thereto. The other end of the reflux pipe is connected to the discharge outlet of the lower chamber. The side wall of the lower chamber is provided with a feed inlet, and a membrane structure fitting is arranged at the feed inlet. A feed pipe and a flow meter are connected to the membrane structure fitting. The opposite side wall is provided with a discharge outlet, and a reflux pipe and a flow meter are connected to the discharge outlet. The other end of the reflux pipe is connected to the feed inlet of the middle chamber, and another discharge outlet is arranged below. One of the two raw material liquids flows into the micro-reactor from the feed inlet of the upper chamber through the flow meter and enters the middle chamber through the distributor. The raw material liquid is mixed with the circulating liquid drawn from the lower chamber in the middle chamber, and then flows into the lower chamber through the distributor. The other raw material is input into the feed pipe by the pump, flows into the micro-reactor from the feed inlet of the lower chamber through the flow meter and the distributor with a hole diameter of 100 μm, and reacts with the slurry from the middle chamber. Part of the reacted slurry flows out of the micro-reactor from the discharge outlet which is located 15 cm below the feed inlet of the lower chamber through the flow meter of the reflux pipe, and the ratio of the flow rate of the circulating liquid input into the reflux pipe to the flow rate of the raw material into the lower chamber is 10. The other part of the reacted slurry flows out of the micro-reactor from the discharge outlet below the lower chamber and flows into the reaction kettle. The materials of the chambers and the inner distributors of the micro-reactor are all stainless steel.

[0037] Example 2

[0038] The micro-reactor of Example 1 is used. The prepared sodium metaaluminate solution with a concentration of 8.48 g / L is input into the lower chamber of the micro-reactor at a flow rate of 205.36 L / h. The prepared aluminum salt solution with a concentration of 3.27 g / L is input into the upper chamber of the micro-reactor at a flow rate of 939.27 L / h, enters the middle chamber through the upper chamber, and then enters the lower chamber to react with the sodium metaaluminate solution. The reaction is carried out at 55.0℃. Part of the mixed di-aluminate solution in the lower chamber is refluxed to the middle chamber, and part of it flows out of the reactor to obtain a γ-Al2O3 precursor suspension and prepare γ-Al2O3. The ratio of the reflux stream to the stream entering the middle chamber from the upper chamber is 5. The pH value of the product slurry is monitored during the preparation, and the specific data are shown in Table 1. Figure 2 .

[0039] Comparative Example

[0040] Using the raw materials in Example 2, but using a mechanically agitated tank reactor including a stirrer and a tank body for a heterogeneous reaction, using a parallel flow dropping method, i.e. two streams of raw materials are dropped into the reactor at the same time, mixed under the action of the stirrer, and the reaction occurs in the process. The product slurry pH during the preparation process is monitored, and the specific data are shown in Table 2. Figure 2 .

[0041] The product slurry pH is a crucial factor affecting the quality of γ-Al2O3 product, and the pH fluctuation has an important influence on the product property repeatability and quality stability. From Table 2, it can be seen that, compared with using a common stirred tank as a reactor, the product slurry pH fluctuation during the preparation process using a microreactor is obviously smaller and more stable. Figure 2

[0042] Of course, the present application can have other various embodiments, and those skilled in the art can make various corresponding changes and modifications according to the present application without departing from the spirit and essence of the present application. However, these corresponding changes and modifications should all belong to the protection scope of the claims of the present application.​

Claims

1. A microreactor suitable for rapid reaction of two liquid phase feedstocks to produce a solid phase product, characterized in that, The application relates to a reactor body, which is divided into three chambers from top to bottom by a first distributor and a second distributor, and is provided with a first feeding port at the top and a first discharging port at the bottom; a second feeding port is arranged on one side of the side wall of the lowermost chamber, and a second discharging port is arranged on the other side; the second feeding port is higher than the second discharging port; the second discharging port is communicated with the middle chamber through a circulating pipeline; the vertical distance between the second feeding port and the second discharging port is greater than or equal to 5 cm; a feeding pipeline and a flowmeter are connected to the first feeding port; a pump and a flowmeter are arranged on the circulating pipeline; a third distributor is arranged at the second feeding port, and a feeding pipeline and a flowmeter are connected to the third distributor; the reactor body is in a straight cylinder type, and the inner diameter is 5-20 cm; the distributor is in a circular disc-shaped hole flow type structure; the hole diameter of the first distributor and the second distributor is 10-1500 mu m; the hole diameter of the third distributor is 0.1-1000 mu m; a mixing strength enhancing component is arranged on the inner wall of the middle chamber; the distributor and the reactor body are sealedly connected through flanges; the inner wall of the reactor body and the distributor are made of stainless steel. ​ ​ 2. The microreactor according to claim 1, wherein, ​ 3. The microreactor according to claim 1, wherein, ​ 4. The microreactor according to claim 1, wherein, ​ 5. The microreactor according to claim 1, wherein, ​ 6. The microreactor suitable for fast reaction of two liquid phase feedstocks to generate solid phase product according to claim 1 or 4, characterized in that, ​ 7. The microreactor according to claim 6, wherein, ​ 8. The microreactor according to claim 6, wherein, ​ 9. The microreactor according to claim 1, wherein, ​ 10. The microreactor suitable for fast reaction of two liquid phase feedstocks to generate solid phase product according to claim 1 or 4, characterized in that, ​ 11. The microreactor suitable for fast reaction of two liquid phase feedstocks to generate solid phase product according to claim 1 or 4, characterized in that, ​

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