Device, application thereof and method for producing pseudo-boehmite by utilizing industrial flue gas

By designing a device containing tower body, air pipe and screen paddle blades, the carbon dioxide in industrial flue gas reacts with alkaline aluminum sources, the problem of difficulty in producing high-purity phthalicite at low concentrations of CO2 is solved, and efficient carbon dioxide capture and high-purity preparation of phthalicite is achieved.

CN119857448APending Publication Date: 2025-04-22CHINA PETROLEUM & CHEMICAL CORP +1
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Patent Information

Application Number
CN202311370244.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-10-20
Publication Date
2025-04-22

AI Technical Summary

Technical Problem

In the prior art, high concentrations of CO2 are required to prepare qualified phthalinite, and it is difficult to directly use industrial flue gas containing low concentrations of carbon dioxide to produce high-purity phthalinite.

Method used

A device is designed, which includes a tower body, a gas pipe and a screen paddle. By reacting carbon dioxide in industrial flue gas with an alkaline aluminum source, a carbonized liquid is obtained, and high-purity pseudothic aluminite is prepared by aging and drying treatment.

Benefits of technology

By strengthening the gas-liquid mass transfer process, the device improves the carbon dioxide capture rate, reduces the generation of heterocensors, improves the purity and crystallinity of phthalidite, and solves the problem that it is difficult to produce high-purity phthalidite at low concentrations of CO2.

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Abstract

The invention relates to the field of pseudo-boehmite preparation, and discloses a device and application thereof, and a method for producing pseudo-boehmite by using industrial flue gas. The device comprises a tower body, a gas pipe arranged in the tower body, a gas inlet and a sieve plate paddle, the gas inlet is connected with one end of a gas pipe and is used for introducing industrial flue gas; the air pipe is provided with at least one sieve plate paddle along the circumferential direction, and is communicated with the sieve plate paddle; and air outlet holes are formed in the sieve plate paddles, so that industrial flue gas emerges from the air outlet holes to react with an alkaline aluminum source. The device provided by the invention is used for preparing pseudo-boehmite by taking industrial flue gas containing low-concentration carbon dioxide as a raw material, and is beneficial to obtaining high-purity pseudo-boehmite.
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Description

Technical Field

[0001] The invention relates to the field of pseudo-boehmite preparation, and in particular to a device and application thereof, and a method for producing pseudo-boehmite by utilizing industrial flue gas. Background Art

[0002] At present, it is urgent to achieve carbon dioxide emission reduction and resource utilization. There is a great enthusiasm for the research on the resource utilization of carbon dioxide. Among them, the preparation of pseudo-boehmite by carbonization is an effective way to capture and utilize CO2. In the process of preparing pseudo-boehmite by carbonization, low concentration of CO2 can easily cause the hydrolysis reaction of sodium aluminate, thereby producing gibbsite impurities. In addition, the traditional carbonization reaction mainly uses the bubble tower as the reaction body. Due to the simple internal structure of the bubble tower, it is only a simple gas-liquid contact reaction, so a high concentration of CO2 is required to participate in the reaction to ensure the preparation of qualified pseudo-boehmite.

[0003] CN106946278A discloses a method for preparing pseudo-boehmite, wherein the reaction tower is a bubbling tower, and the concentration of CO2 gas introduced is 30% to 60%, thereby obtaining qualified pseudo-boehmite. CN111634932A discloses a method for continuously producing pseudo-boehmite, wherein the system includes: a gas-liquid mixing kettle, a decomposition tower, a slurry storage tank, a temperature raising tank, an aging tank, etc. The concentration of CO2 gas introduced is 30% to 100%, thereby obtaining qualified pseudo-boehmite. CN110304644A discloses a method for producing pseudo-boehmite. It uses a high-purity sodium aluminate solution and a carbon dioxide gas with a concentration of 30-50% to react to obtain high-purity pseudo-boehmite, and then uses a hydrothermal high-temperature and high-pressure aging method to deeply remove sodium to obtain high-purity and high-viscosity pseudo-boehmite.

[0004] In the prior art, high concentration of CO2 is generally required to participate in the reaction to ensure the preparation of qualified pseudo-boehmite. Therefore, it is urgent to develop a new method and equipment to achieve the goal of directly using industrial flue gas containing low concentration of carbon dioxide to prepare high-purity pseudo-boehmite. Summary of the invention

[0005] The purpose of the present invention is to overcome the problem in the prior art that it is difficult to produce high-purity pseudo-boehmite directly using industrial flue gas containing low-concentration carbon dioxide as a raw material, and to provide a device and its application and a method for producing pseudo-boehmite using industrial flue gas. The device provided by the present invention is used in preparing pseudo-boehmite using industrial flue gas containing low-concentration carbon dioxide as a raw material, which is conducive to obtaining high-purity pseudo-boehmite.

[0006] In order to achieve the above-mentioned object, the present invention provides a device on one hand, which comprises: a tower body, a gas inlet, a gas pipe disposed inside the tower body, and a sieve plate blade;

[0007] The gas inlet is connected to one end of the gas pipe and is used for the introduction of industrial flue gas;

[0008] The air pipe is provided with at least one sieve plate blade along the circumference and is communicated with the sieve plate blade; the sieve plate blade is provided with an air outlet hole for the industrial flue gas to emerge from the air outlet hole and react with the alkaline aluminum source.

[0009] The second aspect of the present invention provides an application of the device described in the first aspect in producing pseudo-boehmite using industrial flue gas.

[0010] A third aspect of the present invention provides a method for producing pseudo-boehmite using industrial flue gas, the method comprising:

[0011] (1) In the device described in the first aspect, carbon dioxide in industrial flue gas is reacted with an alkaline aluminum source to obtain a carbonized liquid;

[0012] (2) aging the carbonized liquid obtained in step (1) and then drying it;

[0013] Wherein, the concentration of carbon dioxide in the industrial flue gas is 5-40% by volume.

[0014] Preferably, the concentration of carbon dioxide in the industrial flue gas is 10-25% by volume.

[0015] Preferably, the concentration of the alkaline aluminum source solution is 10-50 g / L, preferably 15-40 g / L, more preferably 20-30 g / L.

[0016] Through the above technical solution, the beneficial effects of the present invention include:

[0017] The device provided by the present invention is used to prepare pseudo-boehmite using industrial flue gas containing low-concentration carbon dioxide as a raw material, thereby strengthening the gas-liquid mass transfer process, improving the carbon dioxide capture rate, allowing more carbon dioxide to participate in the reaction, and effectively avoiding the hydrolysis reaction of sodium aluminate, so that the generated pseudo-boehmite has fewer impurity crystals and higher purity, thereby solving the problem that it is difficult to produce high-purity pseudo-boehmite with low-concentration CO2; at the same time, the crystallinity of the generated pseudo-boehmite is improved, and the peptization performance of the generated pseudo-boehmite is enhanced.

[0018] The device provided by the present invention is used to prepare pseudo-boehmite using industrial flue gas containing low-concentration carbon dioxide as a raw material. The operation is simple, the cost is low, and the device is suitable for wide application. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 is a schematic diagram of the device of the present invention;

[0020] Figure 2 is a diagram showing the arrangement of the air outlet holes on a sieve plate blade in the device described in Example 1 of the present invention;

[0021] Figure 3 This is the X-ray diffraction pattern of the pseudo-boehmite prepared in Example 1 of the present invention.

[0022] Description of Reference Numerals

[0023] Figure 1 middle,

[0024] 1. Tower body; 2. Screen plate blades; 3. Air pipe;

[0025] 4. Stirring motor; 5. Gas inlet; 6. Fluid inlet;

[0026] 7. Gas export; 8. Product export. DETAILED DESCRIPTION

[0027] The endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.

[0028] In one aspect, the present invention provides a device, which comprises: a tower body 1, a gas inlet 5, a gas pipe 3 disposed inside the tower body 1, and a sieve plate blade 2;

[0029] The gas inlet 5 is connected to one end of the gas pipe 3 and is used for the introduction of industrial flue gas;

[0030] The air pipe 3 is provided with at least one sieve plate blade 2 along the circumferential direction and is in communication with the sieve plate blade 2; the sieve plate blade 2 is provided with an air outlet hole for the industrial flue gas to escape from the air outlet hole and react with the alkaline aluminum source.

[0031] The device of the present invention improves the mass transfer efficiency of the gas-liquid reaction and the carbon dioxide capture rate by realizing a specific gas-liquid contact mode, so that more carbon dioxide participates in the reaction, and the hydrolysis reaction of sodium aluminate is effectively avoided, so that the generated pseudo-boehmite impurities are reduced and the purity is improved, thereby solving the problem that it is difficult to produce high-purity pseudo-boehmite with low concentration of CO2; at the same time, the crystallinity of the generated pseudo-boehmite is improved, and the peptization performance of the generated pseudo-boehmite is enhanced.

[0032] The present invention has no particular limitation on the size and shape of the tower body 1, which can be appropriately selected according to the application.

[0033] In the present invention, the trachea 3 is connected and communicated with the sieve plate blade 2. The present invention has no particular limitation on the connection method between the trachea 3 and the sieve plate blade 2, and the connection method can be carried out according to conventional methods in the art. For example, the two can be fixedly connected or movably connected.

[0034] The present invention has no particular limitation on the communication method between the air pipe 3 and the sieve plate blade 2, and it can be carried out according to conventional methods in the art, as long as the function of industrial flue gas entering the sieve plate blade 2 through the air pipe 3 and then escaping from the air outlet can be achieved.

[0035] In order to increase the gas-liquid mass transfer rate, preferably, the gas pipe 3 is placed at the center of the tower body 1 .

[0036] The present invention has no particular limitation on the height of the air pipe 3 , which can be higher than the height of the tower body 1 or lower than the height of the tower body 1 , as long as the arrangement of the sieve plate blades 2 on the air pipe 3 meets the experimental requirements, and the present invention has no requirements for this.

[0037] In order to allow industrial flue gas to circulate better in the screen plate blades 2, preferably, the screen plate blades 2 have a hollow structure.

[0038] According to the present invention, preferably, the length of the sieve plate blade 2 is 25-45%, preferably 35-45% of the length of the cross section of the tower body.

[0039] According to the present invention, preferably, the width of the screen plate blade 2 is 20-50% of the length of the screen plate blade 2, preferably 25-45%.

[0040] According to the present invention, preferably, the thickness of the screen plate blade 2 is 30-150 mm, preferably 50-100 mm.

[0041] In the present invention, controlling the size of the screen plate blades 2 is beneficial to the normal operation of the entire system and is more flexible and maneuverable.

[0042] The present invention has no particular limitation on the length direction of the sieve plate blade 2, and it can be set at any angle relative to the downward extension direction of the air pipe 3. Preferably, the length direction of the sieve plate blade 2 is perpendicular to the air pipe 3. This preferred embodiment is beneficial to gas mass transfer during the reaction process.

[0043] In the present invention, the sieve plate blades 2 may be provided in multiple directions along the circumferential direction of the air pipe 3. The sieve plate blades 2 may be at the same height or at different heights, and the present invention has no special limitation on this.

[0044] In the present invention, the reference of “same height” is that the lower surfaces of the screen plate blades are at the same height.

[0045] According to the present invention, preferably, along the circumferential direction, 1 to 4 sieve plate blades 2 are arranged at the same height of the air pipe 3 .

[0046] When two or more sieve plate blades 2 are arranged at the same height of the air pipe 3, they are preferably arranged uniformly along the circumferential direction, that is, the sieve plate blades 2 are arranged at equal angles in the circumferential direction.

[0047] According to the present invention, preferably, at least two sieve plate blades 2 are provided along the extension direction of the gas pipe 3, and preferably the vertical distance between two adjacent sieve plate blades 2 is 15-35%, preferably 20-30% of the height of the tower body 1. This preferred embodiment is conducive to full contact between gas and liquid during the reaction process.

[0048] It should be noted that the vertical distance between two adjacent sieve plate blades 2 refers to the distance between two adjacent sieve plate blades 2 in height, that is, the vertical distance between multiple sieve plate blades 2 arranged circumferentially at the same height is not included.

[0049] In the present invention, the vertical distance between two adjacent sieve plate blades 2 can be the same or different, and the present invention has no requirement for this. Preferably, along the extension direction of the trachea 3, the vertical distance between two adjacent sieve plate blades 2 is the same.

[0050] In the present invention, the “vertical distance” refers to the distance between the upper surface of the sieve plate blade located below and the lower surface of the sieve plate blade located above along the extension direction of the trachea 3 .

[0051] In the present invention, the specific number of the sieve plate blades 2 can be appropriately selected according to the height of the tower body 1. Moreover, in order to make the sieve plate blades play their role better, along the gas flow direction, the sieve plate blades 2 located at the bottom cannot contact the bottom surface of the tower body 1, and need to be at a certain distance from the bottom surface of the tower body 1. Specifically, it can be appropriately adjusted according to actual conditions.

[0052] The shape of the screen plate blade 2 of the present invention can be regular or irregular, for example, the shape of the screen plate blade 2 can be a cuboid, a cube, a quadrangular pyramid, a triangular prism, etc. In order to reduce the resistance during the rotation process, preferably, the shape of the screen plate blade 2 is a quadrangular pyramid and / or a triangular prism, preferably a triangular prism.

[0053] The cross section of the triangular prism screen plate blade of the present invention can be any triangle. According to the present invention, preferably, the cross section of the triangular prism is a right triangle.

[0054] According to the present invention, preferably, the smallest angle of the triangular cross section is 30-45°.

[0055] According to the present invention, preferably, the sieve plate blades are arranged to be rotatable. With this preferred embodiment, the gas-liquid mass transfer process can be effectively strengthened, which is conducive to improving the utilization rate of carbon dioxide, controlling the pH uniformity in the whole tower, and making the pseudo-boehmite crystal phase better and the crystallinity higher. At the same time, the problem of air inlet blockage can be avoided.

[0056] When the screen plate blade 2 is in the shape of a quadrangular pyramid and / or a triangular prism, preferably, the thickness of the screen plate blade gradually decreases in the rotation direction thereof to form a cutting edge.

[0057] By adopting the above preferred embodiment, when the screen plate blades rotate, the thickness of the screen plate blades gradually decreases along the rotation direction of the screen plate blades, which can reduce the resistance during the rotation process. Figure 1 .

[0058] According to the present invention, preferably, along the length direction of the sieve plate blade 2, the apertures of the air outlet holes on the same sieve plate blade 2 increase in sequence in the direction away from the air pipe 3. This preferred embodiment is advantageous in that the generated pseudo-boehmite has a higher crystallinity and a more stable crystal phase.

[0059] It should be noted that, in the present invention, along the length direction of the sieve plate blade 2, the air outlet holes on the same sieve plate blade 2 can be considered to be divided into multiple units, and the air outlet holes in the units farther from the trachea 3 have larger apertures. In each unit, the hole can be one or more, and the number can be unequal. Generally, the number of holes in each unit is 1-5.

[0060] For example, in Example 1, along the length direction of the sieve plate blade 2, the aperture of the air outlet on the same sieve plate blade 2 increases by 2 mm every three holes in the direction away from the trachea 3, so it can be considered that there are three holes in each unit of the air outlet, which can be referred to Figure 2 .

[0061] Preferably, along the length direction of the sieve plate blade 2, the aperture of the air outlet on the same sieve plate blade 2 increases by 1-20 mm, preferably 1-15 mm, in the direction away from the air pipe 3. This preferred embodiment is conducive to the smooth and uniform emergence of CO2, and further conducive to the generated pseudo-boehmite having higher crystallinity and more stable crystal phase.

[0062] The present invention has no special requirements for the aperture distribution of the air outlet holes arranged on the same sieve plate blade 2 along the width direction of the sieve plate blade 2, which can be the same or different. Preferably, along the width direction of the sieve plate blade 2, the apertures of the air outlet holes on the same sieve plate blade 2 are the same.

[0063] According to the present invention, preferably, on the same sieve plate blade 2 , the diameter of the air outlet hole closest to the trachea 3 is 0.25-8% of the length of the sieve plate blade 2 , preferably 0.5-6%.

[0064] In the present invention, the industrial flue gas can emerge from the lower surface of the sieve plate blade 2, or from the upper surface of the sieve plate blade 2, or from the upper and lower surfaces of the sieve plate blade 2 at the same time, and the present invention has no requirements for this. That is, the gas outlet hole of the present invention can be a lower opening, an upper opening, or a through hole. Preferably, the gas outlet hole is an upper opening. Adopting this preferred embodiment is more conducive to the smooth contact reaction between the gas and the liquid.

[0065] The present invention has no particular limitation on the shortest distance between the air outlets, and it is sufficient to ensure that the bubbles can emerge smoothly and do not interfere with each other during the rising process. In order to improve gas-liquid mass transfer, preferably, on the same sieve plate blade 2, the shortest distance between two adjacent air outlets is 1-5% of the length of the sieve plate blade 2, preferably 1-3%.

[0066] In the present invention, on the same screen plate blade, the air outlet holes may be arranged at equal distances or at unequal distances, and the present invention has no requirements for this.

[0067] The present invention has no particular limitation on the number of the air outlet holes and their specific arrangement, which can be appropriately selected according to the specific situation, as long as the above conditions are met.

[0068] In the device of the present invention, only the sieve plate blades 2 may rotate, while the air tube 3 does not rotate; or the sieve plate blades 2 and the air tube 3 may rotate simultaneously.

[0069] The present invention has no particular limitation on the manner in which the screen plate blades are rotated, and the rotation can be achieved by conventional technical means in the art.

[0070] Preferably, the device further comprises a stirring motor 4 connected to the air pipe 3, for controlling the rotation of the sieve plate blade 2. In this preferred embodiment, the sieve plate blade 2 and the air pipe 3 rotate simultaneously.

[0071] In the present invention, the stirring motor 4 includes: Figure 1 The fixed part shown and Figure 1 The part of the rotating shaft not shown in the figure. This is the normal setting.

[0072] Specifically, the stirring motor 4 divides the air pipe 3 into two parts, wherein the air pipe above the stirring motor 4 does not rotate, and the air pipe below the stirring motor 4 and the sieve plate blades rotate together with the rotating shaft.

[0073] According to the present invention, preferably, the device further comprises a gas outlet 7 arranged on the tower body 1 for discharging unreacted industrial flue gas.

[0074] According to the present invention, preferably, the device further comprises a fluid inlet 6 arranged on the tower body 1 for introducing the alkaline aluminum source solution.

[0075] According to the present invention, preferably, the device further comprises a product outlet 8 arranged on the tower body 1 for outputting the carbonized liquid.

[0076] According to a specific embodiment of the present invention, the alkaline aluminum source solution is first introduced from the fluid inlet 6. Then the stirring motor 4 is turned on, the air pipe 3 and the sieve plate blade 2 rotate, and the industrial flue gas is introduced from the gas inlet 5; the industrial flue gas enters the sieve plate blade 2 through the air pipe 3, and then emerges from the gas outlet holes opened on the sieve plate blade 2 to react with the alkaline aluminum source to obtain a carbonized liquid, which is sent out from the product outlet 8 for the next reaction.

[0077] According to a particularly preferred embodiment of the present invention, a device comprises: a tower body 1, a gas pipe 3 disposed inside the tower body 1, a gas inlet 5 and a sieve plate blade 2;

[0078] The gas inlet 5 is connected to one end of the gas pipe 3 and is used for the introduction of industrial flue gas;

[0079] The air pipe 3 is circumferentially provided with at least one sieve plate blade 2 and is connected with the sieve plate blade 2; the sieve plate blade 2 is provided with an air outlet; along the length direction of the sieve plate blade 2, the aperture of the air outlet on the same sieve plate blade 2 increases by 1-15 mm in the direction away from the air pipe 3; on the same sieve plate blade 2, the aperture of the air outlet closest to the air pipe 3 is 0.5-6% of the length of the sieve plate blade 2, which is used for industrial flue gas to emerge from the air outlet and react with the alkaline aluminum source.

[0080] By adopting the above-mentioned preferred embodiment, the air outlet holes on the sieve plate blades are arranged according to a specific pattern, and the aperture of the air outlet holes is controlled within an appropriate range. When the sieve plate blades rotate, the gas-liquid contact will be very sufficient and the reaction will be more complete, which is conducive to the generated pseudo-boehmite with higher crystallinity and more stable crystal phase.

[0081] The second aspect of the present invention provides an application of the device described in the first aspect in producing pseudo-boehmite using industrial flue gas.

[0082] The third aspect of the present invention provides a method for producing pseudo-boehmite using industrial flue gas, characterized in that the method comprises:

[0083] (1) In the device described in the first aspect, carbon dioxide in industrial flue gas is reacted with an alkaline aluminum source to obtain a carbonized liquid;

[0084] (2) aging the carbonized liquid obtained in step (1) and then drying it;

[0085] Wherein, the concentration of carbon dioxide in the industrial flue gas is 5-40% by volume.

[0086] The method provided by the invention can realize the preparation of high-purity pseudo-boehmite by directly using industrial flue gas containing low-concentration carbon dioxide as raw material.

[0087] In the present invention, the concentration of carbon dioxide in the industrial flue gas is 5-40 volume%, preferably 10-25 volume%, for example, 5 volume%, 8 volume%, 10 volume%, 13 volume%, 15 volume%, 18 volume%, 20 volume%, 23 volume%, 25 volume%, 28 volume%, 30 volume%, 33 volume%, 35 volume%, 38 volume%, 40 volume%, and any value in the range formed by any two of these values.

[0088] The present invention has no particular limitation on the composition of the industrial flue gas, and it can be any common industrial flue gas in the art.

[0089] The present invention has no particular limitation on the source of the industrial flue gas, which may be industrial flue gas containing the above-mentioned concentration of carbon dioxide obtained by various methods in the art.

[0090] The specific process of the reaction in step (1) of the present invention in the device described in the first aspect has been described in the first aspect and will not be repeated here.

[0091] The present invention has no particular limitation on the reaction temperature of step (1), which can be selected conventionally in the art. According to the present invention, preferably, the reaction temperature of step (1) is 20-40°C.

[0092] According to the present invention, preferably, the reaction is stopped when the pH value of the reaction solution is 9-11, preferably 9.5-10.5. In this preferred embodiment, it is beneficial to obtain high-purity pseudo-boehmite.

[0093] The present invention does not particularly limit the rotation speed of the sieve plate blade, and can be appropriately selected according to the reaction requirements of step (1). Preferably, the rotation speed of the sieve plate blade is 60-300 r / min. In this preferred embodiment, it is beneficial to accelerate the gas-liquid contact and the reaction process.

[0094] The present invention has no particular limitation on the rate of introduction of industrial flue gas, and can be appropriately selected according to different application scenarios (laboratory, industrial application, etc.) and different reactor sizes.

[0095] When the laboratory is tested, preferably, the flow rate of the industrial flue gas is 0.3-2L / min, preferably 0.8-1.5L / min, such as 0.3L / min, 0.4L / min, 0.5L / min, 0.6L / min, 0.7L / min, 0.8L / min, 0.9L / min, 1L / min, 1.1L / min, 1.2L / min, 1.3L / min, 1.4L / min, 1.5L / min, 1.6L / min, 1.7L / min, 1.8L / min, 1.9L / min, 2L / min, and any value in the range formed by any two of these numerical values. Under this preferred embodiment, it is conducive to more sufficient gas-liquid contact and more complete reaction. It is conducive to the generated pseudo-boehmite crystallinity to be higher and the crystalline phase to be more stable.

[0096] Preferably, the industrial flue gas is cooled to below 30° C. before being introduced from the gas inlet. In this preferred embodiment, the generated pseudo-boehmite has fewer impurity crystals and a higher crystallinity.

[0097] According to the present invention, preferably, the concentration of the alkaline aluminum source solution is 10-50 g / L, preferably 15-40 g / L, more preferably 20-30 g / L, such as 10 g / L, 15 g / L, 20 g / L, 25 g / L, 30 g / L, 35 g / L, 40 g / L, 45 g / L, 50 g / L, and any value in the range formed by any two of these values. Under this preferred embodiment, it is beneficial to generate less pseudo-boehmite impurities, higher purity, higher crystallinity, and faster reaction time.

[0098] The inventors found during the research process that when the concentration of the alkaline aluminum source solution is higher than the above range, sodium aluminate is prone to undergo hydrolysis reaction to produce some gibbsite impurity crystals.

[0099] The present invention has a wide range of solvent types for the alkaline aluminum source solution, which can be a conventional choice in the art. Preferably, the solvent in the alkaline aluminum source solution is water.

[0100] The present invention has a wide range of choices for the basic aluminum source, which can be a conventional choice in the art. Preferably, the basic aluminum source is sodium metaaluminate.

[0101] According to the present invention, preferably, the aging conditions in step (2) include: a temperature of 50-120° C., preferably 90-120° C.; and a time of 60-300 minutes, preferably 180-300 minutes.

[0102] According to the present invention, preferably, the drying conditions in step (2) include: a temperature of 70-120° C., preferably 70-110° C.; and a time of 120-300 minutes, preferably 180-240 minutes.

[0103] Preferably, the method further comprises: washing and filtering the aged product before drying. The above-mentioned washing and filtering is a conventional operation in the art, and the specific method is well known to those skilled in the art, and the present invention will not be described in detail here.

[0104] The present invention will be described in detail below through examples.

[0105] In the following examples, the crystallinity and grain size of the samples were determined by X-ray powder diffraction (XRD) using RIPP145-90 and RIPP146-90 standard methods (see "Petrochemical Analysis Methods" (RIPP Test Methods) edited by Yang Cuiding et al., Science Press, published in 1990);

[0106] The CO2 capture rate was determined using an infrared gas analyzer produced by Xilinzi Technology Development Co., Ltd., instrument model: XLZ-1090;

[0107] The specific surface area and total pore volume of the sample were determined by the BET method, using the ASAP2405N V1.01 automatic adsorption instrument from Micromeritics, USA. The specific surface area (S BET ), determine the volume of N2 adsorbed by the sample when the relative pressure p / p0=0.98, and measure the total pore volume;

[0108] Determination of sample peptization index (DI): Weigh 5g of pseudo-boehmite (dry basis) with a sieve size of less than 200 mesh and place it in a 250mL conical flask, add appropriate amount of deionized water and stir, add appropriate amount of hydrochloric acid, stir for a certain period of time, let it stand and settle for 24 hours, pour off the upper suspension, dry, roast, weigh the sample mass (W), and calculate the peptization index DI = (5-W) / 5.

[0109] Example 1

[0110] Use Figure 1 The device shown is a device, which includes: a tower body 1, an air pipe 3 placed at the center of the tower body 1, a sieve plate blade 2 with a hollow structure arranged inside the tower body 1, a stirring motor 4 arranged on the upper part of the air pipe 3 and above the outside of the tower body 1, a gas inlet 5 connected to the upper end of the air pipe 3, a gas outlet 7 arranged above the outside of the tower body 1, a fluid inlet 6 arranged on the tower body 1, and a product outlet 8 arranged on the tower body 1. The tower body 1 is cylindrical, with a height of 150 cm and a bottom diameter of 100 cm.

[0111] The sieve plate blades are arranged to be rotatable; two sieve plate blades 2 are fixedly arranged at the same height along the circumference of the air pipe 3, and the sieve plate blades 2 are arranged at equal angles in the circumference; three sieve plate blades 2 are arranged equidistantly along the extension direction of the air pipe 3, and the vertical distance between two adjacent sieve plate blades 2 is 300mm; along the gas flow direction, the distance between the lowest sieve plate blade 2 and the bottom surface of the tower body 1 is 10cm. The length direction of the sieve plate blade 2 is perpendicular to the air pipe 3; the air pipe 3 is connected to the sieve plate blade 2.

[0112] The length of the sieve plate blade 2 is 40% of the diameter of the tower cross section, and the width of the sieve plate blade 2 is 45% of the length of the sieve plate blade 2; the height of the sieve plate blade 2 is 100 mm; the shape of the sieve plate blade 2 is a triangular prism; the triangular cross section of the triangular prism is a right triangle; the angle of the smallest angle of the right triangle is 30°. The thickness of the sieve plate blade 2 gradually decreases in its rotation direction to form a cutting edge.

[0113] The sieve plate paddle 2 is provided with 80 upper openings. Along the width direction of the sieve plate paddle 2, the apertures of the air outlet holes on the same sieve plate paddle 2 are the same, with a total of 4 rows, 20 in each row; along the length direction of the sieve plate paddle 2, the apertures of the air outlet holes on the same sieve plate paddle 2 increase by 2 mm every 3 holes in the direction away from the trachea 3, such as Figure 2 As shown; on the same sieve plate paddle 2, the diameter of the air outlet hole which is closest to the trachea 3 and is 0.3 cm is 8 mm; on the same sieve plate paddle, the air outlet holes are arranged equidistantly, and the shortest distance between two adjacent air outlet holes is 6 mm.

[0114] At room temperature, a sodium aluminate aqueous solution with a concentration of 30 g / L is introduced into the above device, and then industrial flue gas (composed of 25 volume % CO2 + 3 volume % O2 + 72 volume % N2) with a temperature of 25°C is introduced at a flow rate of 0.9 L / min, and the rotation speed of the sieve plate blade is set to 150 r / min. The industrial flue gas emerges from the air outlet of the sieve plate blade and contacts and reacts with the sodium aluminate. When the pH of the solution drops to 10.4, the reaction is stopped and the material is discharged to obtain a carbonized liquid. An infrared gas analyzer is set at the gas outlet to calculate the CO2 capture rate. The CO2 capture rate is shown in Table 2.

[0115] The obtained carbonized liquid was aged at an aging temperature of 90° C. for 180 minutes. The aged product was washed and filtered, and then dried at 90° C. for 180 minutes to obtain pseudo-boehmite powder S1. The physicochemical properties of pseudo-boehmite powder S1 are shown in Table 1.

[0116] The XRD pattern of the obtained pseudo-boehmite is given as an example, Figure 3As shown, it can be seen that the obtained sample has obvious characteristic peaks of pseudo-boehmite, almost no impurity peaks, unit cell 4.1, and crystallinity 87%, which shows that high-purity pseudo-boehmite is prepared.

[0117] Example 2

[0118] A device, comprising: a tower body 1, an air pipe 3 placed at the center of the tower body 1, a hollow sieve plate blade 2 arranged inside the tower body 1, a stirring motor 4 arranged on the upper part of the air pipe 3 and above the outside of the tower body 1, a gas inlet 5 connected to the upper end of the air pipe 3, a gas outlet 7 arranged above the outside of the tower body 1, a fluid inlet 6 arranged on the tower body 1, and a product outlet 8 arranged on the tower body 1. The tower body 1 is a cube, with a height of 140 cm and a bottom length of 60 cm.

[0119] The sieve plate blade is configured to be rotatable; one sieve plate blade 2 is provided at the same height along the circumference of the air pipe 3; five sieve plate blades 2 are provided equidistantly along the extension direction of the air pipe 3, and the vertical distance between two adjacent sieve plate blades 2 is 35 mm; along the gas flow direction, the distance between the lowest sieve plate blade 2 and the bottom surface of the tower body 1 is 8 cm. The length direction of the sieve plate blade 2 is perpendicular to the air pipe 3; the air pipe 3 is connected to the sieve plate blade 2.

[0120] The length of the sieve plate blade 2 is 40% of the length of the tower cross section, the width of the sieve plate blade 2 is 40% of the length of the sieve plate blade 2; the height of the sieve plate blade 2 is 100 mm; the length direction of the sieve plate blade 2 is perpendicular to the air pipe 3; the shape of the sieve plate blade 2 is a triangular prism; the triangular cross section of the triangular prism is a right triangle; the angle of the smallest angle in the triangle is 45°. The thickness of the sieve plate blade gradually decreases in its rotation direction to form a cutting edge.

[0121] The sieve plate paddle 2 is provided with 60 upper openings. Along the width direction of the sieve plate paddle 2, the apertures of the air outlet holes on the same sieve plate paddle 2 are the same, with a total of 4 rows and 15 holes in each row; along the length direction of the sieve plate paddle 2, the apertures of the air outlet holes on the same sieve plate paddle 2 increase by 2 mm every 2 holes in the direction away from the trachea 3; on the same sieve plate paddle 2, the aperture of the air outlet hole that is closest to the trachea 3 and is 0.5 cm is 6 mm; on the same sieve plate paddle, the air outlet holes are arranged equidistantly, and the shortest distance between two adjacent air outlet holes is 4 mm.

[0122] At room temperature, a sodium aluminate aqueous solution with a concentration of 20 g / L is introduced into the above device, and then industrial flue gas (composed of 14 volume % CO2 + 3 volume % O2 + 83 volume % N2) with a temperature of 30°C is introduced at a flow rate of 1.2 L / min, and the rotation speed of the sieve plate blade is set to 300 r / min. The industrial flue gas emerges from the air outlet of the sieve plate blade and contacts and reacts with the sodium aluminate. When the pH of the solution drops to 10.2, the reaction is stopped and the material is discharged to obtain a carbonized liquid. An infrared gas analyzer is set at the gas outlet to calculate the CO2 capture rate. The CO2 capture rate is shown in Table 2.

[0123] The obtained carbonized liquid was aged at an aging temperature of 100° C. for 180 minutes. The aged product was washed and filtered, and then dried at 90° C. for 180 minutes. Pseudo-boehmite powder S2 was obtained. The physicochemical properties of the pseudo-boehmite powder S2 are shown in Table 1.

[0124] Example 3

[0125] The method of Example 1 was followed, except that the 80 air outlet holes on the sieve plate blade 2 had the same aperture of 12 mm, to obtain pseudo-boehmite powder S3. The physicochemical properties of pseudo-boehmite powder S3 are shown in Table 1. The CO2 capture rate is shown in Table 2.

[0126] Comparative Example 1

[0127] The method of Example 2 was followed, except that a conventional bubbling bed reactor was used in the process of preparing the carbonized liquid to obtain pseudo-boehmite powder D1. The physicochemical properties of pseudo-boehmite powder D1 are shown in Table 1.

[0128] The conventional bubbling bed reactor comprises a tower body, a gas distribution plate arranged on the bottom cross section of the tower body, an air inlet at the bottom of the tower, a gas outlet at the upper part of the tower body and a product outlet at the bottom of the tower. The industrial flue gas is introduced through the lower air inlet, dispersed by the gas distribution plate, and reacts with the sodium aluminate aqueous solution in the tower body. The obtained carbonized liquid is sent out from the product outlet for the next experiment. An infrared gas analyzer is arranged at the gas outlet to calculate the CO2 capture rate. The CO2 capture rate is shown in Table 2. The tower body size is the same as that of Example 2.

[0129] The conventional bubbling bed reactor has a general effect on carbon dioxide mass transfer, a low carbon dioxide utilization rate, and the holes of the gas distributor and the air inlet at the bottom of the tower are easily clogged during the reaction.

[0130] Comparative Example 2

[0131] The conventional bubbling bed reactor of Comparative Example 1 is used, except that

[0132] At room temperature, a sodium aluminate aqueous solution with a concentration of 40 g / L was introduced into a conventional bubbling bed reactor, and then industrial flue gas (composed of 40% by volume CO2 + 3% by volume O2 + 57% by volume N2) with a temperature of 30°C was introduced at a flow rate of 1 L / min to contact and react with the sodium aluminate. When the pH of the solution dropped to 10.5, the reaction was stopped and the material was discharged to obtain a carbonized liquid. An infrared gas analyzer was set at the gas outlet to calculate the CO2 capture rate, and the CO2 capture rate is shown in Table 2.

[0133] The obtained carbonized liquid was aged at an aging temperature of 90°C for 180 minutes. The aged product was washed and filtered, and then dried at 90°C for 180 minutes to obtain pseudo-boehmite powder D2. The physicochemical properties of pseudo-boehmite powder D2 are shown in Table 1.

[0134] Table 1

[0135]

[0136] It can be seen from the results in Table 1 that when the device of the present invention is used to prepare pseudo-boehmite using industrial flue gas containing low concentration of carbon dioxide as raw material, the obtained pseudo-boehmite has higher crystallinity, higher peptization index, larger specific surface area, larger total pore volume and larger grain size, and has better application effect in the field of catalyst preparation.

[0137] Table 2

[0138]

[0139] Note: CO2 capture rate = (CO2 concentration in initial industrial flue gas - CO2 concentration in tail gas) / CO2 concentration in initial industrial flue gas × 100%

[0140] It can be seen from the results in Table 2 that the CO2 capture rate can be greatly increased by using the device of the present invention, more carbon dioxide participates in the reaction, and the hydrolysis reaction of sodium aluminate is effectively avoided, so that the generated pseudo-boehmite impurities are reduced, the purity is improved, and the performance is better.

[0141] The preferred embodiments of the present invention are described in detail above, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention.

Claims

1. A device, comprising: A tower body (1), a gas inlet (5), a gas pipe (3) disposed inside the tower body (1), and a sieve plate blade (2); The gas inlet (5) is connected to one end of the gas pipe (3) and is used for the introduction of industrial flue gas; The air pipe (3) is provided with at least one sieve plate blade (2) along the circumferential direction and is in communication with the sieve plate blade (2); the sieve plate blade (2) is provided with an air outlet hole for the industrial flue gas to escape from the air outlet hole and react with the alkaline aluminum source.

2. The device according to claim 1, wherein: The sieve plate blade 2 has a hollow structure; Preferably, the length of the sieve plate blade (2) is 25-45% of the cross-sectional length of the tower body, preferably 35-45%; Preferably, the width of the screen plate blade (2) is 20-50%, preferably 25-45% of the length of the screen plate blade (2); Preferably, the thickness of the screen plate blade (2) is 30-150 mm, preferably 50-100 mm; Preferably, along the circumferential direction, 1 to 4 sieve plate blades (2) are arranged at the same height of the air pipe (3); Preferably, at least two sieve plate blades (2) are provided along the extension direction of the air pipe (3), and preferably the vertical distance between two adjacent sieve plate blades (2) is 15-35% of the height of the tower body (1).

3. The device according to claim 1, wherein: The screen plate blade (2) is in the shape of a quadrangular pyramid and / or a triangular prism, preferably a triangular prism; Preferably, the cross section of the triangular prism is a right triangle; Preferably, the smallest angle of the triangular cross section is 30-45°; Preferably, the screen plate blade (2) is configured to be rotatable; Preferably, the thickness of the screen plate blade gradually decreases in the rotation direction thereof to form a cutting edge.

4. The device according to any one of claims 1 to 3, wherein: Along the length direction of the sieve plate blade (2), the apertures of the air outlet holes on the same sieve plate blade (2) increase in sequence in a direction away from the trachea (3); Preferably, along the length direction of the sieve plate blade (2), the diameter of the air outlet holes on the same sieve plate blade (2) increases by 1-20 mm, preferably 1-15 mm, in a direction away from the trachea (3); Preferably, on the same sieve plate blade (2), the diameter of the air outlet hole closest to the trachea (3) is 0.25-8% of the length of the sieve plate blade (2), preferably 0.5-6%; Preferably, on the same sieve plate blade (2), the shortest distance between two adjacent air outlet holes is 1-5% of the length of the sieve plate blade (2).

5. The device according to any one of claims 1 to 4, wherein: The device also includes a stirring motor (4) connected to the air pipe (3) and used to control the rotation of the sieve plate blade (2); Preferably, the device further comprises a gas outlet (7) arranged on the tower body (1) for discharging unreacted industrial flue gas; Preferably, the device further comprises a fluid inlet (6) disposed on the tower body (1) for introducing a basic aluminum source solution; Preferably, the device further comprises a product outlet (8) arranged on the tower body (1) for outputting the carbonized liquid.

6. Use of the device according to any one of claims 1 to 5 in producing pseudo-boehmite using industrial flue gas.

7. A method for producing pseudo-boehmite using industrial flue gas, characterized in that: The method includes: (1) In the device according to any one of claims 1 to 5, carbon dioxide in industrial flue gas is reacted with an alkaline aluminum source to obtain a carbonized liquid; (2) aging the carbonized liquid obtained in step (1) and then drying it; Wherein, the concentration of carbon dioxide in the industrial flue gas is 5-40% by volume.

8. The method according to claim 7, wherein: Step (1) comprises: S1, flowing alkaline aluminum source solution into the fluid inlet; S2. The industrial flue gas is introduced from the gas inlet, passes through the gas pipe, and emerges from the gas outlet holes of the sieve plate blades to react with the alkaline aluminum source solution to obtain a carbonized liquid.

9. The method according to claim 7 or 8, wherein: The reaction temperature in step (1) is 20-40°C; Preferably, the reaction is stopped when the pH value of the reaction solution is 9-11, preferably 9.5-10.5; Preferably, the rotation speed of the screen plate blade is 60-300r / min; Preferably, the flow rate of the industrial flue gas is 0.3-2 L / min, preferably 0.8-1.5 L / min; Preferably, the concentration of carbon dioxide in the industrial flue gas is 10-25% by volume; Preferably, the concentration of the alkaline aluminum source solution is 10-50 g / L, preferably 15-40 g / L, more preferably 20-30 g / L; Preferably, the alkaline aluminum source is sodium metaaluminate.

10. The method according to any one of claims 7 to 9, wherein: The aging conditions in step (2) include: a temperature of 50-120° C., preferably 90-120° C.; a time of 60-300 minutes, preferably 180-300 minutes; Preferably, the drying conditions in step (2) include: a temperature of 70-120° C., preferably 70-110° C.; and a drying time of 120-300 minutes, preferably 180-240 minutes.

Citation Information

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