Preparation method of high-performance special mineral admixture

Through the combination of low-temperature activation and microwave treatment, high-performance special mineral blends are prepared, which solves the problems of high energy consumption and high carbon emissions, improves the performance and stability of cement-based materials, and simplifies the production process.

CN120441219APending Publication Date: 2025-08-08CCCC SHANGHAI HARBOR ENG DESIGN & RES INST
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Patent Information

Application Number
CN202510548762.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-28
Publication Date
2025-08-08

AI Technical Summary

Technical Problem

The existing preparation methods of high-performance special mineral blends have problems with high energy consumption and high carbon emissions, and the production process is complicated, making it difficult to meet the stability requirements of large-scale industrial production.

Method used

Low-temperature activation technology is adopted to form a mixed material by selecting mineral raw materials for pretreatment, and the first activation reaction is carried out in the low-temperature activation equipment, followed by ball milling, and then a second microwave activation to form a high-performance special mineral blend.

Benefits of technology

It significantly improves the compressive strength and chloride ion permeability of cement-based materials, while maintaining early strength in low-temperature environments, reducing energy consumption and carbon emissions, and simplifying the production process.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a preparation method of a high-performance special mineral admixture. The preparation method comprises the following steps: selecting mineral raw materials; pretreating the mineral raw materials to form a mixed material; putting the mixed material into low-temperature activation equipment, and carrying out first activation reaction treatment to form a first semi-finished product; carrying out ball milling treatment on the first semi-finished product to form a second semi-finished product; and performing second activation reaction treatment on the second semi-finished product to form the high-performance special mineral admixture. In the application, when the high-performance special mineral admixture prepared by two times of low-temperature activation treatment is applied to the cement-based material, the compressive strength and the chloride ion penetration resistance can be remarkably improved, meanwhile, the workability of the cement-based material is not reduced, and the early strength performance in a low-temperature environment is also very excellent.
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Description

Technical Field

[0001] The present application belongs to the field of construction engineering technology, and specifically relates to a method for preparing a high-performance special mineral admixture. Background Art

[0002] In today's booming construction industry, high-performance specialty mineral admixtures are crucial for improving the performance of cement-based materials and reducing cement usage. They not only optimize concrete properties but also align with green building concepts. However, current technologies still face numerous challenges in their preparation.

[0003] Existing high-performance specialty mineral admixtures are often prepared using high-temperature activation technology. This method, foremost among these, is characterized by its significant energy consumption. For example, the production of high-performance admixtures using common slag requires calcining the slag at temperatures between 800°C and 1000°C. The continuous operation of high-temperature kilns consumes significant amounts of energy, including coal and natural gas, significantly increasing production costs. This drawback is becoming increasingly prominent in today's increasingly energy-scarce world.

[0004] This is accompanied by a serious carbon emissions problem. The combustion of fossil fuels during the high-temperature activation process releases vast amounts of carbon dioxide. It's estimated that a medium-sized admixture manufacturer using traditional high-temperature processes could emit tens of thousands of tons of carbon dioxide annually, exacerbating global warming and seriously contradicting my country's "dual carbon" goals.

[0005] In addition, the preparation process in the existing technology is generally complicated. Some solutions for preparing special mineral admixtures from industrial waste require multiple rounds of crushing and screening of the raw materials, followed by acid and alkali pretreatment, followed by high-temperature calcination, and finally multiple grinding. Complex processes lengthen the production cycle and reduce efficiency. Any slight deviation in operation will affect product quality, making it difficult to meet the requirements of industrial large-scale production for product stability. Therefore, an innovative preparation method is urgently needed to break through the difficulties. A solution based on low-temperature activation technology has emerged, which is expected to solve the problems of existing technologies and promote the green development of the industry. Summary of the Invention

[0006] In view of the shortcomings or deficiencies of the above-mentioned prior art, the technical problem to be solved by this application is a method for preparing high-performance special mineral admixtures.

[0007] To solve the above technical problems, this application is implemented through the following technical solutions:

[0008] This application proposes a method for preparing a high-performance special mineral admixture, comprising the following steps:

[0009] Selection of mineral raw materials;

[0010] Pre-treating the mineral raw materials to form a mixed material;

[0011] placing the mixed material in a low-temperature activation device for a first activation reaction to form a first semi-finished product;

[0012] ball milling the first semi-finished product to form a second semi-finished product;

[0013] After the second semi-finished product is subjected to a second activation reaction treatment, a high-performance special mineral admixture is formed.

[0014] Optionally, the above-mentioned pre-processing of the mineral raw materials to form a mixed material includes: removing impurities from the mineral raw materials.

[0015] Optionally, the pretreatment process includes: using screening equipment to perform screening, magnetic separation and other operations in sequence, controlling the particle size of the mineral raw material to be 0.1mm-5mm, and the magnetic impurity content to be lower than 0.8%. The above settings can lay a good foundation for subsequent reactions.

[0016] Optionally, the above-mentioned pre-treating of the mineral raw material to form a mixed material further includes: uniformly mixing the pre-treated mixed material with an activator.

[0017] Optionally, the activator includes: an organic liquid activator or a biological enzyme activator, wherein, when the organic liquid activator is used, the dosage of the organic liquid activator is 5%-10% of the mass of the mixed material; when the biological enzyme activator is used, the dosage of the biological enzyme activator is 0.1%-0.4% of the mass of the mixed material.

[0018] Optionally, in the above-mentioned first activation reaction treatment, it includes: placing the mixed material in a low-temperature activation device with a temperature control accuracy of up to ±5°C, in a temperature range of 40°C to 60°C, at a stirring rate of 150r / min to 220r / min, the activation reaction lasts for 1h to 2h to form a first semi-finished product. The above-mentioned low-temperature activation greatly reduces energy consumption.

[0019] Optionally, the ball milling of the first semi-finished product includes: grinding the first semi-finished product for 2-3 hours using a ball mill, and collecting a second semi-finished product with a particle size of 50-200 nm. The ball milling device may be a ball mill or other equipment.

[0020] Optionally, the second activation treatment includes: using microwave equipment to perform a second activation treatment on the second semi-finished product to form a high-performance special mineral admixture, wherein the active substance content is not less than 90%; the microwave power of the microwave equipment is 300W-1000W, the reaction temperature is 60℃-90℃, and the particles are fully dispersed, and when preparing cement-based materials, the particles will not agglomerate. The microwave treatment time is 10min-20min. The high-performance special mineral admixture prepared by this method, when applied to cement-based materials, can significantly improve the compressive strength and resistance to chloride ion penetration, while not reducing the workability of the cement-based materials, and the early strength performance in low-temperature environments is also excellent.

[0021] Optionally, the low-temperature activation equipment is provided with a spiral stirring blade and / or a gas distributor to ensure that the mixed material is heated evenly and reacts fully during the activation process. The temperature control accuracy of the equipment is within ±5°C.

[0022] Optionally, the mineral raw materials are electrolytic manganese slag, blast furnace water-quenched slag, and waste ceramic powder compounded in a certain proportion, and the content of electrolytic manganese slag in the compounding proportion is not less than 50%.

[0023] Compared with the existing technology, this application has the following technical effects:

[0024] When the high-performance special mineral admixture of this application is applied to cement-based materials, the compressive strength of the cement-based materials can be increased by more than 20% and the chloride ion penetration resistance can be increased by more than 40% after 28 days of standard curing. In addition, in a low temperature environment (-5℃-10℃), the early strength (3-day compressive strength) of the cement-based materials can reach more than 70% of the design strength. DETAILED DESCRIPTION

[0025] The following will be combined with the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the embodiments described are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments of the present application, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of this application.

[0026] In one embodiment of the present application, a method for preparing a high-performance specialty mineral admixture comprises the following steps:

[0027] Step 1: Select mineral raw materials;

[0028] Step 2: Pre-treating the mineral raw materials to form a mixed material;

[0029] Step 3: placing the mixed material in a low-temperature activation device for a first activation reaction to form a first semi-finished product;

[0030] Step 4: ball milling the first semi-finished product to form a second semi-finished product;

[0031] Step five: performing a second activation reaction on the second semi-finished product to form a high-performance special mineral admixture.

[0032] Wherein, in the above step 1, the mineral raw materials are electrolytic manganese slag, blast furnace water-quenched slag, and waste ceramic powder compounded in a certain proportion, and the content of electrolytic manganese slag in the compounding proportion is not less than 50%.

[0033] In the above-mentioned step 2, the above-mentioned pre-treatment of the mineral raw materials to form a mixed material includes: removing impurities from the mineral raw materials. Specifically, screening equipment can be used to perform screening, magnetic separation and other operations in sequence to control the particle size of the mineral raw materials to be 0.1mm-5mm, and the magnetic impurity content to be less than 0.8%; more preferably, the particle size of the mineral raw materials is controlled to be 0.5mm-5mm, and the magnetic impurity content is less than 0.75%; more preferably, the particle size of the mineral raw materials is controlled to be 1mm-5mm, and the magnetic impurity content is less than 0.7%; more preferably, the particle size of the mineral raw materials is controlled to be 2mm-5mm, and the magnetic impurity content is less than 0.7%; more preferably, the particle size of the mineral raw materials is controlled to be 2mm-4mm, and the magnetic impurity content is less than 0.6%; more preferably, the particle size of the mineral raw materials is controlled to be 2.5mm-4mm, and the magnetic impurity content is less than 0.5%; more preferably, the particle size of the mineral raw materials is controlled to be 3mm-5mm, and the magnetic impurity content is less than 0.4%. Through the above settings, a good reaction foundation can be laid for subsequent reactions.

[0034] Furthermore, after the above-mentioned impurity removal treatment, the pretreated mixed material is further mixed evenly with an activator.

[0035] The activator includes an organic liquid activator or a bio-enzyme activator. When the organic liquid activator is used, the amount of the organic liquid activator is 5%-10% of the mass of the mixed material; when the bio-enzyme activator is used, the amount of the bio-enzyme activator is 0.1%-0.4% of the mass of the mixed material. The organic liquid activator can be mainly a polyol liquid activator.

[0036] In step three, the mixture is placed in a low-temperature activation device, and the activation reaction is continued for 1 to 2 hours at a stirring rate of 150 to 220 r / min within a temperature range of 40°C to 60°C to form a first semi-finished product. The above-mentioned low-temperature activation greatly reduces energy consumption. The low-temperature activation device is equipped with a spiral stirring blade and / or a gas distributor. The mixture is placed in a low-temperature activation device equipped with special structures such as a spiral stirring blade and a gas distributor. This configuration allows the temperature control accuracy of the low-temperature activation device to reach ±5°C.

[0037] In the above step 4, the second semi-finished product with a particle size of 50-200nm is collected by grinding with a ball mill for 2h-3h. Further preferably, a ball mill or other equipment can be used for grinding; further preferably, the second semi-finished product with a particle size of 80-200nm is collected by grinding with a ball mill for 2h-2.5h; further preferably, the second semi-finished product with a particle size of 100-200nm is collected by grinding with a ball mill for 2h-2.5h; further preferably, the second semi-finished product with a particle size of 100-180nm is collected by grinding with a ball mill for 2h-2.5h; further preferably, the second semi-finished product with a particle size of 100-150nm is collected by grinding with a ball mill for 2h-2.5h; further preferably, the second semi-finished product with a particle size of 100-120nm is collected by grinding with a ball mill for 2h-2.5h. The second semi-finished product after the above treatment can be used for the subsequent second activation treatment.

[0038] In the above step five, it includes: using microwave equipment to perform a second activation treatment on the second semi-finished product to form a high-performance special mineral admixture, wherein the active substance content is not less than 90%; the microwave power of the microwave equipment is 300W-1000W, the reaction temperature is 60℃-90℃, and the microwave treatment time is 10min-20min.

[0039] The following is a detailed description of different embodiments of the present application.

[0040] Example 1

[0041] (1) Preparation of mineral raw materials: Electrolytic manganese slag and blast furnace water-quenched slag with a mass ratio of 3:2 are selected as mineral raw materials, and pre-processed using a vibrating screen and a magnetic separator to ensure that the particle size of the mineral raw materials is 0.1-3 mm and the magnetic impurity content is less than 0.5%.

[0042] (2) Preparation of activator: Select polyol liquid activator as the main activator, and mix the activator solution and pretreated mineral raw materials in a mass ratio of 1:10.

[0043] (3) Low-temperature activation (first activation treatment): The mixed material is placed in a low-temperature activation device with a spiral stirring blade inside, with a temperature control accuracy of ±2°C. The activation reaction is carried out at 60°C and a stirring rate of 150 r / min for 2 hours. After the reaction is completed, the first semi-finished product is obtained.

[0044] (4) Grinding: Grind the first semi-finished product in a ball mill for 2 h, and collect particles with a particle size of 50-100 nm in an air classifier to obtain a second semi-finished product;

[0045] (5) Microwave treatment (second activation treatment): The second semi-finished product is placed in a microwave treatment device, and the microwave power is set to 300 W, the reaction temperature is set to 90° C., and the treatment time is set to 20 min to obtain a high-performance special mineral admixture.

[0046] Example 2

[0047] (1) Preparation of mineral raw materials: Electrolytic manganese slag and waste ceramic powder with a mass ratio of 5:5 were selected as mineral raw materials, and pre-processed using a vibrating screen and a magnetic separator to ensure that the particle size of the mineral raw materials was 0.2-5 mm and the magnetic impurity content was less than 0.8%.

[0048] (2) Preparation of activator: Select alkyd synthetic liquid activator as the main activator, and mix the activator solution and pretreatment raw materials at a mass ratio of 1:20.

[0049] (3) Low-temperature activation (first activation treatment): The above-mentioned mixed material is placed in a low-temperature activation device with a spiral stirring blade inside, with a temperature control accuracy of ±5°C. The activation reaction is carried out at 40°C and a stirring rate of 220 r / min for 3 hours. After the reaction is completed, the first semi-finished product is obtained.

[0050] (4) Grinding: Grind the first semi-finished product in a ball mill for 3 h, and collect particles with a particle size of 50-200 nm in an air classifier to obtain a second semi-finished product;

[0051] (5) Microwave treatment (second activation treatment): The second semi-finished product is placed in a microwave treatment device, and the microwave power is set to 1000 W, the reaction temperature is set to 60° C., and the treatment time is set to 10 min to obtain a high-performance special mineral admixture.

[0052] Example 3

[0053] (1) Preparation of mineral raw materials: Electrolytic manganese slag, blast furnace water-quenched slag and waste ceramic powder with a mass ratio of 3:2:1 were selected as mineral raw materials. They were pre-treated using a vibrating screen and a magnetic separator to ensure that the particle size of the mineral raw materials was 0.3-5 mm and the magnetic impurity content was less than 0.4%.

[0054] (2) Preparation of activator: Select multi-enzyme bio-enzyme activator as the main activator, and mix the activator solution and pre-treated raw materials at a mass ratio of 1:1000.

[0055] (3) Low-temperature activation (first activation treatment): The mixed material is placed in a low-temperature activation device with a spiral stirring blade inside, with a temperature control accuracy of ±5°C. The activation reaction is carried out at 60°C and a stirring rate of 150 r / min for 1 hour. After the reaction is completed, the first semi-finished product is obtained.

[0056] (4) Grinding: Grind the first semi-finished product in a ball mill for 2 h, and collect particles with a size of 100-200 nm in an air classifier to obtain a second semi-finished product;

[0057] (5) Microwave treatment (second activation treatment): The second semi-finished product is placed in a microwave treatment device, and the microwave power is set to 500 W, the reaction temperature is set to 70° C., and the treatment time is set to 15 min to obtain a high-performance special mineral admixture.

[0058] The high-performance mineral admixture prepared in the above embodiment was added to cement-based materials to prepare cement mortar, wherein the mass ratio of PO 42.5 grade cement to the high-performance mineral admixture was 1:1, and pure PO 42.5 grade cement was set as a control group. The relevant performance indicators are shown in Table 1 below.

[0059] Table 1 Performance optimization degree of cement mortar prepared with high-performance mineral admixtures compared with the control group

[0060]

[0061] In this application, when the high-performance special mineral admixture prepared by two low-temperature activation treatments is applied to cement-based materials, the compressive strength of the cement-based materials can be increased by more than 20% and the chloride ion penetration resistance can be increased by more than 40% after 28 days of standard curing. In addition, in a low temperature environment (-5℃-10℃), the early strength (3-day compressive strength) of the cement-based materials can reach more than 70% of the design strength.

[0062] The above description of the embodiments is intended to facilitate understanding and use by those skilled in the art.

[0063] The above embodiments are intended only to illustrate the technical solutions of the present application and are not intended to limit the present application. The present application is described in detail with reference to the preferred embodiments. It should be understood by those skilled in the art that the technical solutions of the present application may be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present application and should be included within the scope of the claims of the present application.

Claims

1. A method for preparing a high-performance special mineral admixture, characterized in that: The following steps are involved: Selection of mineral raw materials; Pre-treating the mineral raw materials to form a mixed material; placing the mixed material in a low-temperature activation device for a first activation reaction to form a first semi-finished product; ball milling the first semi-finished product to form a second semi-finished product; After the second semi-finished product is subjected to a second activation reaction treatment, a high-performance special mineral admixture is formed.

2. The method for preparing high-performance special mineral admixture according to claim 1, characterized in that: The above-mentioned pre-processing of the mineral raw materials to form a mixed material includes: removing impurities from the mineral raw materials.

3. The method for preparing high-performance special mineral admixture according to claim 2, characterized in that: The pretreatment process includes: using screening equipment to perform screening, magnetic separation and other operations in sequence, controlling the particle size of the mineral raw materials to be 0.1mm-5mm and the magnetic impurity content to be lower than 0.8%.

4. The method for preparing high-performance special mineral admixture according to claim 1, characterized in that: The above-mentioned pre-treating of the mineral raw materials to form a mixed material further includes: uniformly mixing the pre-treated mixed material with an activator.

5. The method for preparing high-performance special mineral admixture according to claim 4, characterized in that: The activator includes: an organic liquid activator or a biological enzyme activator, wherein, when the organic liquid activator is used, the dosage of the organic liquid activator is 5%-10% of the mass of the mixed material; when the biological enzyme activator is used, the dosage of the biological enzyme activator is 0.1%-0.4% of the mass of the mixed material.

6. The method for preparing high-performance special mineral admixture according to claim 1, characterized in that: In the above-mentioned first activation reaction treatment, it includes: placing the mixed material in a low-temperature activation device, in a temperature range of 40°C to 60°C, at a stirring rate of 150r / min to 220r / min, the activation reaction continues for 1h to 2h to form a first semi-finished product.

7. The method for preparing high-performance special mineral admixture according to claim 1, characterized in that: The ball milling treatment of the first semi-finished product includes: grinding the first semi-finished product with a ball mill for 2 hours to 3 hours, and collecting the second semi-finished product with a particle size in the range of 50-200 nm.

8. The method for preparing high-performance special mineral admixture according to claim 1, characterized in that: In the above-mentioned second activation treatment, it includes: using microwave equipment to perform a second activation treatment on the second semi-finished product to form a high-performance special mineral admixture, wherein the active substance content is not less than 90%; the microwave power of the microwave equipment is 300W-1000W, the reaction temperature is 60℃-90℃, and the microwave treatment time is 10min-20min.

9. The method for preparing high-performance special mineral admixture according to claim 8, characterized in that: The low-temperature activation equipment is internally provided with a spiral stirring blade and / or a gas distributor.

10. The method for preparing a high-performance special mineral admixture according to any one of claims 1 to 9, characterized in that: The mineral raw materials are electrolytic manganese slag, blast furnace water-quenched slag, and waste ceramic powder, which are compounded in a certain proportion, and the content of the electrolytic manganese slag in the compounding proportion is not less than 50%.