A continuous negative pressure filling material mineralization co2 device and method

Abstract

The application discloses a continuous negative pressure filling material mineralization CO2 device and method, and belongs to the field of carbon neutralization. The device is composed of a CO2 gas source conveying system, a mineralization reaction system and an intelligent control monitoring system. The method is to place a demolded prefabricated cementing material in a vacuum box, use a vacuum pump to vacuumize the vacuum box, maintain negative pressure for 5-10 minutes, and close the vacuum pump. Then, open the gas switch valve, make CO2 gas enter the vacuum box, until the pressure of the vacuum box recovers to 0.1 MPa±0.05, continue mineralization for 5-15 minutes, close the gas switch valve, complete a complete negative pressure mineralization step, repeat the vacuumizing-pressure maintaining-CO2 filling-mineralization step for 2-5 times, and complete the continuous negative pressure filling material mineralization CO2. The continuous negative pressure filling material mineralization CO2 device of the application is flexible, widely applicable, can realize the purpose of quickly mineralizing CO2 of the cementing material in a short time, and the internal mineralization degree of the cementing material is relatively uniform.

Description

Technical Field

[0001] This invention belongs to the field of carbon neutralization, specifically relating to a device and method for mineralizing CO2 using continuous negative pressure filling materials. Background Technology

[0002] CO2 mineralization and sequestration technology, which converts CO2 into stable carbonate minerals to achieve CO2 sequestration, is considered one of the key approaches to addressing global climate change and achieving carbon neutrality.

[0003] Traditional CO2 mineralization methods are mostly pressure-based, which promote the reaction between CO2 and metal ions in minerals by increasing the gas injection pressure, thus accelerating the carbonate formation process. Although this method is widely used, numerous laboratory experiments have shown that it has many drawbacks. During pressure-based mineralization, the transfer efficiency of CO2 gas into the cementitious material is slow, typically reaching the mineralization peak after 10 hours. This results in a high degree of mineralization on the outside of the cementitious material and a lower degree of mineralization inside, leading to uneven mineralization. Furthermore, when the gas injection pressure exceeds the strength of the cementitious material, it can easily cause damage. Therefore, exploring a new mineralization method to avoid these problems while achieving rapid and efficient CO2 mineralization and sequestration is of great significance.

[0004] Based on this, the present invention proposes a device and method for continuous negative pressure filling material mineralization of CO2. The device is flexible and has a wide range of applications. By repeatedly vacuuming, maintaining pressure, filling with CO2, and mineralizing, it completes the continuous negative pressure filling material mineralization of CO2, achieving the goal of rapid CO2 mineralization of cementitious materials in a short time. Moreover, the degree of mineralization inside the cementitious materials is relatively uniform, and it has broad application prospects. Summary of the Invention

[0005] Purpose of the invention: To address the shortcomings of existing technologies, this invention provides a device and method for continuous negative pressure filling material to mineralize CO2. This device is flexible, has a wide range of applications, and can achieve the purpose of rapid CO2 mineralization of cementitious materials in a short time, with a relatively uniform degree of mineralization inside the cementitious materials.

[0006] Technical solution: To achieve the above objectives, the technical solution adopted by this invention is as follows:

[0007] On one hand, this invention provides a continuous negative pressure filling material mineralization CO2 device, which consists of three parts: a CO2 gas source delivery system, a mineralization reaction system, and a temperature and pressure intelligent control and monitoring system.

[0008] The CO2 gas supply system includes CO2 cylinders, gas switching valves, and gas connection pipelines connected in sequence.

[0009] The mineralization reaction system includes a vacuum chamber and a vacuum pump, which are connected by rubber hoses;

[0010] The intelligent temperature and pressure control and monitoring system includes a temperature control and monitoring unit, a humidity control and monitoring unit, a pressure control and monitoring unit, and an analytical electronic balance installed inside the vacuum chamber, which transmit data to the data monitoring and analysis platform through a signal transmission channel;

[0011] The pre-formulated cementitious material is placed on an analytical electronic balance inside the vacuum chamber.

[0012] Preferably, the side length of the vacuum box is 1000mm~6000mm.

[0013] Preferably, the temperature inside the vacuum chamber is controlled between room temperature and 100°C. Excessive temperature will cause the hydration products in the cementitious material to decompose.

[0014] Preferably, the temperature control monitoring unit, humidity control monitoring unit, pressure control monitoring unit, and analytical electronic balance are all arranged inside the vacuum chamber, which facilitates real-time and accurate monitoring and control of changes in temperature, humidity, pressure, and mineralization within the vacuum chamber.

[0015] On the other hand, the present invention also provides a method for a continuous negative pressure filling material mineralization CO2 device, the steps of which are as follows:

[0016] a. Place the pre-prepared cementitious material on the analytical electronic balance inside the vacuum chamber, use a vacuum pump to evacuate the vacuum chamber, maintain the negative pressure for 5-10 minutes, and then turn off the vacuum pump;

[0017] b. Open the CO2 cylinder valve to allow CO2 gas to enter the vacuum chamber until the pressure inside the vacuum chamber returns to 0.1±0.05 MPa. Continue mineralization for 5-15 minutes to ensure the mineralization reaction proceeds fully. Observe the real-time mineralization status using an analytical electronic balance. Close the CO2 cylinder valve to complete one complete negative pressure mineralization step.

[0018] c. Repeat steps a and b to complete the vacuuming, negative pressure, pressure holding, CO2 filling, and mineralization steps 2-5 times to achieve continuous negative pressure filling of the material and CO2 mineralization.

[0019] Preferably, the precast cementitious material includes cement-based materials, alkali-activated materials, and cementitious filling materials with an age of 1-28 days after demolding.

[0020] Preferably, the precast cementitious material can be of any shape, not limited to cuboids, cylinders, spheres, etc., and a suitable shape can be selected according to actual needs.

[0021] Preferably, the edge length of the precast cementitious material is 20mm to 1000mm.

[0022] Preferably, in step a, the vacuum is drawn to a negative pressure of -0.1 ± 0.05 MPa to ensure that the air in the reactor is discharged as much as possible.

[0023] Beneficial effects: The continuous negative pressure filling material mineralization CO2 device and method provided by the present invention have the following advantages compared with the prior art:

[0024] 1. A vacuum pump is used to evacuate the vacuum chamber to a negative pressure, which facilitates the diffusion of CO2 gas into the interior of the cementitious material, resulting in a more uniform degree of mineralization inside the cementitious material.

[0025] 2. Negative pressure mineralization can effectively avoid the problem of damage to cementitious materials caused by excessively high injected gas pressure;

[0026] 3. By repeating the vacuuming-pressure holding-CO2 filling-mineralization steps, the purpose of rapidly mineralizing CO2 in cementitious materials in a short time can be achieved. In the embodiments of the present invention, the mineralization rate of 0.71-1.42% was achieved in 10-75 minutes.

[0027] 4. The vacuum chamber can accommodate pre-formed cementitious materials in shapes such as cuboids, cylinders, and spheres, making the continuous negative pressure filling material mineralization CO2 device flexible and applicable to a wide range of fields. Attached Figure Description

[0028] Figure 1 This is a schematic diagram of the structure of the continuous negative pressure filling material mineralization CO2 device of the present invention;

[0029] In the diagram: 1—CO2 cylinder; 2—gas switch valve; 3—gas connection pipeline; 4—pressure control monitoring unit; 5—temperature control monitoring unit; 6—humidity control monitoring unit; 7—rubber hose; 8—vacuum pump; 9—data monitoring and analysis platform; 10—vacuum box; 11—precast cementitious material.

[0030] Figure 2 The diagram shows the spraying of phenolphthalein indicator on the cross-section of the sample before and after mineralization of the material obtained in Example 2. (a) is a schematic diagram of the spraying of phenolphthalein indicator on the cross-section of the sample before mineralization in Example 2; (b) is a schematic diagram of the spraying of phenolphthalein indicator on the cross-section of the sample after mineralization in Example 2. Detailed Implementation

[0032] The embodiments of the present invention will be further described below with reference to the accompanying drawings:

[0033] like Figure 1As shown, the present invention discloses a continuous negative pressure filling material mineralization CO2 device, comprising three parts: a CO2 gas source delivery system, a mineralization reaction system, and an intelligent control and monitoring system. The CO2 gas source delivery system consists of a CO2 cylinder 1, a gas switching valve 2, and a gas connection pipeline 3 connected in sequence. The mineralization reaction system includes a vacuum chamber 10 and a vacuum pump 8, connected by a rubber hose 7. The intelligent control and monitoring system comprises a temperature control monitoring unit 5, a humidity control monitoring unit 6, a pressure control monitoring unit 4, and an analytical electronic balance 12 installed within the vacuum chamber 10, transmitting data to a data monitoring and analysis platform 9 via a signal transmission channel.

[0034] The vacuum chamber 10 has a size range of 1000mm to 6000mm. The temperature, humidity and pressure inside the vacuum chamber 10 are regulated by the temperature control and monitoring unit 5, the humidity control and monitoring unit 6 and the pressure monitoring and control unit 4 arranged on the inside, wherein the temperature is maintained between room temperature and 100℃.

[0035] The pre-formed cementitious material is placed on the analytical electronic balance 12 inside the vacuum chamber 10, and the mineralization degree of the pre-formed cementitious material can be calculated based on the real-time measurement data of the analytical electronic balance 12.

[0036] A test method for a continuous negative pressure filling material mineralization CO2 device, the steps of which are as follows:

[0037] a. Place the pre-prepared cementitious material 11 on the analytical electronic balance 12 inside the vacuum chamber 10, use the vacuum pump 8 to evacuate the vacuum chamber 10, maintain the negative pressure for 5-10 minutes, and then turn off the vacuum pump 8.

[0038] b. Open valve 2 of CO2 cylinder 1 to allow CO2 gas to enter vacuum chamber 10 until the pressure inside vacuum chamber 10 returns to 0.1±0.05 MPa. Continue mineralization for 5-15 minutes. Observe the real-time mineralization status using electronic balance 12. Close valve 2 of CO2 cylinder 1 to complete one complete negative pressure mineralization step.

[0039] c. Repeat steps a and b to complete the vacuuming, negative pressure, pressure holding, CO2 filling, and mineralization steps 2-5 times to achieve continuous negative pressure filling of the material and CO2 mineralization.

[0040] The vacuum pump 8 draws the vacuum chamber 10 to a negative pressure of -0.1 ± 0.05 MPa;

[0041] The precast cementitious material 11 is a cement-based material, alkali-activated material, cementitious filling material, etc., with an age of 1d-28d after demolding. It can be any shape, not limited to cuboid, cylinder, sphere, etc., and its edge length is 20mm~1000mm.

[0042] The present invention will be further described below with reference to embodiments. The present invention can be better understood from the following embodiments. However, those skilled in the art will readily understand that the specific material ratios, process conditions, and results described in the embodiments are for illustrative purposes only and should not, and will not, limit the present invention as described in detail in the claims.

[0043] Example 1 (Control Group):

[0044] This embodiment aims to study the mineralization degree of precast cementitious materials under conditions without vacuuming.

[0045] A test method for a continuous negative pressure filling material mineralization CO2 device, the steps of which are as follows:

[0046] a. After demolding for 3 days, the precast cementitious material 11, which is cube-shaped and has an edge length of 70.7 mm, is placed into a vacuum box 10 with an edge length of 1000 mm, without vacuuming.

[0047] b. Open the gas switch valve 2 of CO2 cylinder 1 to allow CO2 gas to enter the vacuum chamber 10, mineralize for 10 minutes, observe the real-time mineralization status through the analytical electronic balance 12, and close the gas switch valve 2 of CO2 cylinder 1 to complete a complete negative pressure mineralization step.

[0048] c. Repeat steps a and b.

[0049] In this embodiment, the mineralization rate reached 0.05% in the first mineralization, 0.11% in the second mineralization, and 0.23% in the third mineralization.

[0050] Example 2:

[0051] This embodiment aims to study the effect of maintaining a negative pressure of -0.15 MPa in a vacuum chamber for 5 minutes on mineralization.

[0052] A test method for a continuous negative pressure filling material mineralization CO2 device, the steps of which are as follows:

[0053] a. After demolding for 3 days, the precast cementitious material 11, which is cube-shaped and has an edge length of 70.7 mm, is placed into a vacuum chamber 10 with an edge length of 1000 mm. The vacuum chamber is evacuated to a negative pressure of -0.15 MPa using a vacuum pump 8, and the negative pressure is maintained for 5 minutes. Then the vacuum pump 8 is turned off.

[0054] b. Open the gas switch valve 2 of CO2 cylinder 1 to allow CO2 gas to enter the vacuum chamber 10 until the pressure inside the vacuum chamber 10 returns to 0.1MPa. Continue mineralization for 10 minutes. Observe the real-time mineralization status through the analytical electronic balance 12. Close the gas switch valve 2 of CO2 cylinder 1 to complete a complete negative pressure mineralization step.

[0055] c. Repeat steps a and b to complete the vacuuming, negative pressure, pressure holding, CO2 filling, and mineralization steps three times to achieve continuous negative pressure filling of the material and CO2 mineralization.

[0056] In this embodiment, the mineralization rate reached 0.36% in the first mineralization, 0.71% in the second mineralization, and 1.12% in the third mineralization. Therefore, it has good prospects for widespread application.

[0057] Example 3:

[0058] This embodiment aims to study the effect of different pressures on mineralization. The difference from Embodiment 2 is that the vacuum chamber is evacuated to a negative pressure of -0.06 MPa and maintained at the negative pressure for 5 minutes.

[0059] A test method for a continuous negative pressure filling material mineralization CO2 device, the steps of which are as follows:

[0060] a. After demolding for 3 days, the precast cementitious material 11, which is cube-shaped and has an edge length of 70.7 mm, is placed into a vacuum chamber 10 with an edge length of 1000 mm. The vacuum chamber is evacuated to a negative pressure of -0.06 MPa using a vacuum pump 8, and the negative pressure is maintained for 5 minutes. Then the vacuum pump 8 is turned off.

[0061] b. Open the gas switch valve 2 of CO2 cylinder 1 to allow CO2 gas to enter the vacuum chamber 10 until the pressure inside the vacuum chamber 10 returns to 0.1MPa. Continue mineralization for 10 minutes. Observe the real-time mineralization status through the analytical electronic balance 12. Close the gas switch valve 2 of CO2 cylinder 1 to complete a complete negative pressure mineralization step.

[0062] c. Repeat steps a and b to complete the vacuuming, negative pressure, pressure holding, CO2 filling, and mineralization steps three times to achieve continuous negative pressure filling of the material and CO2 mineralization.

[0063] In this embodiment, the mineralization rate reached 0.20% in the first mineralization, 0.55% in the second mineralization, and 0.88% in the third mineralization. Therefore, it has good prospects for widespread application.

[0064] Example 4:

[0065] This embodiment aims to study the effect of different negative pressure times on mineralization. Specifically, under the condition a, the vacuum chamber is evacuated to a negative pressure of -0.15 MPa and maintained at negative pressure for 10 min.

[0066] A test method for a continuous negative pressure filling material mineralization CO2 device, the steps of which are as follows:

[0067] a. After demolding for 3 days, the precast cementitious material 11, which is cube-shaped and has an edge length of 70.7 mm, is placed into a vacuum chamber 10 with an edge length of 1000 mm. The vacuum chamber is evacuated to a negative pressure of -0.15 MPa using a vacuum pump 8, and the negative pressure is maintained for 10 minutes. Then the vacuum pump 8 is turned off.

[0068] b. Open the gas switch valve 2 of CO2 cylinder 1 to allow CO2 gas to enter the vacuum chamber 10 until the pressure inside the vacuum chamber 10 returns to 0.1MPa. Continue mineralization for 20 minutes. Observe the real-time mineralization status through the analytical electronic balance 12. Close the gas switch valve 2 of CO2 cylinder 1 to complete a complete negative pressure mineralization step.

[0069] c. Repeat steps a and b to complete the vacuuming, negative pressure, pressure holding, CO2 filling, and mineralization steps three times to achieve continuous negative pressure filling of the material and CO2 mineralization.

[0070] In this embodiment, the mineralization rate reached 0.38% in the first mineralization, 0.73% in the second mineralization, and 1.17% in the third mineralization.

[0071] The implementation case results show that reducing the vacuum level significantly reduces mineralization efficiency, while extending the mineralization time (from 5 min to 10 min) does not significantly improve mineralization efficiency. Since further reducing the vacuum level beyond -0.1 MPa is difficult and costly, Implementation Case Two represents the optimal mineralization conditions: the vacuum chamber was evacuated to -0.15 MPa and maintained at this negative pressure for 5 min. The mineralization results were as follows: 0.36% mineralization in the first mineralization; 0.71% in the second; and 1.12% in the third. (Comparison) Figure 2 (a) and Figure 2 (b) shows a schematic diagram of the phenolphthalein indicator sprayed on the middle section of the sample before and after mineralization of the sample obtained in Example 2. It can be seen that after negative pressure mineralization, the middle section of the sample is basically colorless after the phenolphthalein indicator is applied, indicating that CO2 penetrates into the interior of the cementitious material. The mineralization degree on the surface of the specimen is relatively uniform.

[0072] The technical means disclosed in this invention are not limited to those disclosed in the above embodiments, but also include technical solutions composed of any combination of the above technical features. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principles of this invention, and these improvements and modifications are also considered within the scope of protection of this invention.

Claims

1. A continuous negative pressure filling material mineralization CO2 device, characterized in that, The device consists of three parts: a CO2 gas supply system, a mineralization reaction system, and a temperature and pressure intelligent control and monitoring system. The CO2 gas supply system includes a CO2 cylinder (1), a gas switch valve (2), and a gas connection pipeline (3) connected in sequence. The mineralization reaction system includes a vacuum chamber (10) and a vacuum pump (8), which are connected by a rubber hose (7), and the pre-made gelling material is placed inside the vacuum chamber (10); The temperature and pressure intelligent control and monitoring system includes a temperature control and monitoring unit (5), a humidity control and monitoring unit (6), a pressure control and monitoring unit (4), and an analytical electronic balance (12) installed in a vacuum chamber (10), which transmits data to the data monitoring and analysis platform (9) through a signal transmission channel. The pre-formed cementitious material is placed on an analytical electronic balance (12) inside the vacuum chamber (10).

2. The continuous negative pressure filling material mineralization CO2 device according to claim 1, characterized in that, The side length of the vacuum box (10) is 1000mm~6000mm.

3. The continuous negative pressure filling material mineralization CO2 device according to claim 1, characterized in that, The temperature inside the vacuum chamber (10) is controlled between room temperature and 100°C.

4. A method for mineralizing CO2 using the continuous negative pressure filling material device according to any one of the preceding claims, characterized in that, Includes the following steps: a. Place the pre-made cementitious material in the vacuum chamber (10) and analyze it on the electronic balance (12). Use the vacuum pump (8) to evacuate the vacuum chamber (10) and maintain the negative pressure for 5-10 minutes. Then turn off the vacuum pump (8). b. Open the CO2 cylinder switch valve (2) to allow CO2 gas to enter the vacuum chamber (10) until the pressure inside the vacuum chamber (10) returns to 0.1±0.05 MPa. Continue mineralization for 5-15 minutes to ensure the mineralization reaction proceeds fully. Observe the real-time mineralization status using an analytical electronic balance (12). Close the CO2 cylinder switch valve (2) to complete a full negative pressure mineralization step. c. Repeat steps a and b to complete the vacuuming, negative pressure, pressure holding, CO2 filling, and mineralization steps 2-5 times to achieve continuous negative pressure filling of the material and CO2 mineralization.

5. The method of the continuous negative pressure filling material mineralization CO2 device according to claim 4, characterized in that, The precast cementitious material includes cement-based materials, alkali-activated materials, or cementitious filling materials with an age of 1-28 days after demolding.

6. The method of the continuous negative pressure filling material mineralization CO2 device according to claim 4, characterized in that, The precast cementitious material can be of any shape, not limited to cuboids, cylinders or spheres.

7. The method of the continuous negative pressure filling material mineralization CO2 device according to claim 4, characterized in that, The edge length of the precast cementitious material is 20mm~1000mm.

8. The method of the continuous negative pressure filling material mineralization CO2 device according to claim 4, characterized in that, In step a, a vacuum is drawn to a negative pressure of -0.1 ± 0.05 MPa.

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