Gelling material based on sulfonated mud and preparation method thereof

Abstract

The invention relates to the technical field of building materials, and discloses a cementing material based on sulfonated mud and a preparation method thereof. The binding material based on sulfonated mud comprises the following components in parts by mass: 30-50 parts of sulfonated mud, 20-30 parts of an active auxiliary material, 10-20 parts of fly ash and 3-8 parts of an active exciting agent. The preparation method of the binding material based on sulfonated mud comprises the following steps: pretreatment of raw materials: dehydrating the sulfonated mud to control the water content, and grinding the active auxiliary materials and fly ash; uniformly stirring and mixing the active auxiliary material, the fly ash, the active exciting agent and the sulfonated mud according to a mass ratio; aging the uniformly mixed material to obtain a primary gel material; according to the technical scheme, the waste sulfonated mud is converted into the cementing material with excellent performance. On one hand, the environmental pollution problem of sulfonated mud is solved from the source, and resource utilization of waste is achieved; on the other hand, the production energy consumption and cost of the cementing material are greatly reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of building materials, and in particular to a sulfonated slurry-based gelling material and a preparation method thereof. Background Art

[0002] With the booming global construction industry, demand for cementitious materials continues to rise. While traditional cementitious materials, such as cement, play a key role in the construction industry, their production is accompanied by significant energy consumption. Statistics show that producing one ton of cement requires approximately 1.5 tons of limestone, 0.3 tons of clay, and 120-150 kilograms of standard coal, while also emitting approximately one ton of carbon dioxide, undoubtedly placing a heavy burden on the ecological environment.

[0003] Furthermore, the ecological environment is also impacted by the large amounts of sulfonated mud produced during operations such as oil extraction and geological exploration. This sulfonated mud has a complex composition, containing large amounts of clay minerals, barite, organic treatment agents, and various metal ions. If not properly handled and dumped, it not only consumes valuable land resources but can also cause serious pollution to surrounding soil and water bodies due to natural factors such as rainwater erosion. Therefore, finding a technical solution that can effectively utilize sulfonated mud while reducing the energy consumption and environmental impact of cementitious material production has become a critical challenge for the industry. Summary of the Invention

[0004] The present invention provides a sulfonated slurry-based cementitious material and a preparation method thereof, so as to solve the above-mentioned technical problems of high energy consumption and great environmental impact in the production of cementitious materials in the prior art.

[0005] According to a first aspect of the present invention, there is provided a sulfonated mud-based cementitious material comprising the following components in parts by mass:

[0006] 30-50 parts of sulfonated mud, 20-30 parts of active auxiliary materials, 10-20 parts of fly ash, and 3-8 parts of active activator.

[0007] Preferably, the active auxiliary material includes one or more of slag, cement, silica fume, carbide slag, steel slag, red mud and biochar-based materials.

[0008] Preferably, the active stimulant includes one or more of an alkaline stimulant, an acidic stimulant, a salt stimulant and a biological agent, wherein multiple components constitute a composite stimulant.

[0009] Preferably, the alkaline activator includes one or more of sodium hydroxide, potassium hydroxide and sodium silicate.

[0010] Preferably, the sulfonated mud-based cementitious material comprises:

[0011] 5-10 parts of gypsum or lime.

[0012] According to a second aspect of the present invention, there is provided a method for preparing a sulfonated slurry-based cementitious material as described above, comprising the following steps:

[0013] S1. Raw material pretreatment: dehydration of sulfonated slurry to control moisture content, grinding of active ingredients and fly ash;

[0014] S2 mixing: The active material, fly ash, active activator and dehydrated sulfonated slurry are stirred and mixed uniformly in a mass ratio;

[0015] S3. Aging treatment: Aging the uniformly mixed material to obtain a preliminary gel material.

[0016] Preferably, in the dehydration treatment of the sulfonated mud to control the water content in step S1, the sulfonated mud is pre-screened to remove impurities, and the sulfonated mud is dehydrated to a water content of less than 30%.

[0017] Preferably, in the grinding treatment of active auxiliary materials and fly ash in step S1, the specific surface area of ​​the grinding treatment material is 400-500m 2 / kg; and / or

[0018] In step S4, the specific surface area of ​​the grinding material is 500-600m 2 / kg.

[0019] Preferably, step S2 is carried out in a mixer at a rotation speed of 80-120 r / min; and / or

[0020] Gypsum or lime is added into the mixer according to the mass ratio and mixed with the materials.

[0021] Preferably, the method for preparing the sulfonated mud-based gelling material comprises the following steps:

[0022] S4. Secondary grinding treatment: grinding the preliminary gel material to further increase the specific surface area of ​​the preliminary gel material to obtain a gel material product.

[0023] The technical solution of this invention, through a unique formulation and preparation process, transforms waste sulfonated mud into a high-performance cementitious material. This not only addresses the environmental pollution problem of sulfonated mud at its source, but also significantly reduces the energy consumption and cost of cementitious material production, promoting the green and sustainable development of the building materials industry. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1The present invention is a schematic flow chart of a method for preparing a sulfonated slurry-based cementitious material in an embodiment. DETAILED DESCRIPTION

[0025] It should be noted that, in the absence of conflict, the embodiments and features of the embodiments of the present invention can be combined with each other. The present invention will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0026] In order to enable those skilled in the art to better understand the solutions of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts should fall within the scope of protection of the present invention.

[0027] It should be noted that the terms "first," "second," and the like in the present invention are used to distinguish similar objects and are not necessarily used to describe a particular order or precedence. It should be understood that the terms used in this manner are interchangeable where appropriate for the embodiments of the present invention described herein. In addition, the terms "including," "having," and any variations thereof are intended to cover non-exclusive inclusions. For example, a process, method, system, product, or apparatus comprising a series of steps or elements is not necessarily limited to those steps or elements explicitly listed, but may include other steps or elements not explicitly listed or inherent to such process, method, product, or apparatus.

[0028] It should be understood that when an element (such as a layer, film, region, or substrate) is described as being "on" another element, the element may be directly on the other element or intervening elements may be present. Moreover, in the present invention, when an element is described as being "connected" to another element, the element may be "directly connected" to the other element or "connected" to the other element through a third element.

[0029] Example 1

[0030] Please refer to Figure 1 This embodiment provides a method for preparing a sulfonated slurry-based gelling material, comprising the following steps:

[0031] S1. Raw material pretreatment: dehydration of sulfonated slurry to control moisture content, grinding of active ingredients and fly ash;

[0032] S2 mixing: The active material, fly ash, active activator and dehydrated sulfonated slurry are stirred and mixed uniformly in a mass ratio;

[0033] S3. Aging: The mixed material is aged to obtain a preliminary gel material. The mixed material is transferred to an aging bin for 2-3 days. During the aging process, the various components in the material react slowly with the active stimulant to form a preliminary gel structure, further improving the performance of the gel material.

[0034] S4. Secondary grinding treatment: grinding the preliminary gel material to further increase the specific surface area of ​​the preliminary gel material to obtain a gel material product.

[0035] In one embodiment, in the dehydration treatment of the sulfonated mud to control the water content in step S1, the sulfonated mud is pre-screened to remove impurities in the sulfonated mud, and then the sulfonated mud is dehydrated to a water content of less than 30%. A combination of mechanical centrifugal dehydration and drying can be used to quickly reduce the water content of the sulfonated mud to less than 30% for subsequent processing.

[0036] In one embodiment, in the grinding treatment of active auxiliary materials and fly ash in step S1, slag and fly ash are respectively put into a ball mill for grinding treatment, and the specific surface area of ​​the grinding material is adjusted to 400-500m by precisely controlling the grinding time and speed. 2 / kg, fully stimulating the potential activity of the raw materials.

[0037] In one embodiment, in step S2, the dehydrated sulfonated mud, slag, fly ash, gypsum, and alkaline activator are sequentially added to a twin-shaft forced mixer, and the mixer is stirred at a speed of 80-120 r / min for 10-20 minutes to ensure that the raw materials are fully mixed and evenly mixed, creating good conditions for subsequent chemical reactions. The active auxiliary material is preferably slag, the active activator is preferably an alkaline activator, and gypsum can be replaced with lime. The mass parts of each raw material are: 30-50 parts of sulfonated mud, 20-30 parts of slag, 10-20 parts of fly ash, 3-8 parts of alkaline activator, and 5-10 parts of gypsum. Among them, the sulfonated mud serves as the core raw material; the slag serves as an auxiliary cementitious material. Its rich active ingredients can synergize with other raw materials to improve the performance of the cementitious material. Fly ash can not only improve the working performance of the cementitious material, but also increase its later strength. Gypsum and lime mainly play the role of regulating the setting time. The alkaline activator includes one or more combinations of sodium hydroxide, potassium hydroxide, and sodium silicate, and its function is to activate the activity of sulfonated mud and slag and accelerate the chemical reaction process.

[0038] Specifically, the selection of raw materials is based on:

[0039] Although sulfonated slurry is a waste product, the clay minerals and organic treatment agents within it can participate in the cementation reaction under the right conditions. Slag has potential hydraulic properties and, under the action of alkaline activators, can produce a large amount of hydration products, enhancing the strength of the cementitious material. The spherical particle structure of fly ash improves the workability of the cementitious material, while its active ingredients can continue to participate in the reaction at a later stage. Gypsum is added to precisely control the setting time of the cementitious material, ensuring sufficient operating time during construction.

[0040] In one embodiment, in step S4, the aged material is again ground in a high-efficiency ball mill to increase its specific surface area to 500-600m 2 / kg, making the particles finer and fully releasing the activity. This produces a gelling material product. Furthermore, the gelling material product is packaged using automated packaging equipment, and the weight of each bag can be set to 25kg, 50kg, etc. according to market demand, facilitating storage and transportation of the gelling material product.

[0041] The sulfonated mud-based cementitious material and its preparation method of the present invention focus on how to process the sulfonated mud produced by industries such as oil extraction and geological exploration, and innovatively convert it into a high-performance cementitious material. The unique preparation method is elaborated in detail, opening up a new path for the green development of building materials. The sulfonated mud-based cementitious material and its preparation method have environmental benefits: they achieve zero emissions of sulfonated mud, converting it from a pollutant into a useful resource, effectively alleviating environmental pressure; and the heavy metal ions in the sulfonated mud are wrapped by slag glass and solidified through a silicate network, and the leaching toxicity is lower than the national standard. It has economic benefits: due to the utilization of discarded sulfonated mud, the production cost of cementitious materials is greatly reduced; after calculation, compared with traditional cement, the cost of the cementitious material of the present invention can be reduced by 30-50 yuan per ton, which has significant economic benefits. Performance advantages: Laboratory tests and actual engineering applications show that the cementitious material prepared by the present invention has excellent compressive strength and durability. Its 28-day compressive strength can reach 40-50 MPa, and its water-resistance grade reaches P8 or above, which can meet the needs of various construction projects, especially hydraulic structures and underground projects with high durability requirements.

[0042] Example 2

[0043] This embodiment provides a sulfonated mud-based cementitious material.

[0044] 1. Raw material formula: 30 parts of sulfonated mud, 25 parts of slag, 15 parts of fly ash, 8 parts of gypsum, and 5 parts of sodium hydroxide.

[0045] 2. Preparation process: Strictly follow the above preparation method. First, dehydrate the sulfonated slurry to reduce its water content to 28%. Then grind the slag and fly ash to a specific surface area of ​​420m 2 / kg. During the mixing and stirring stage, the mixer speed is controlled at 100r / min and the stirring time is 15 minutes. The aging treatment is carried out in a constant temperature and humidity aging chamber, with the temperature controlled at 25°C and the humidity controlled at 60%. Finally, the powder is ground to a specific surface area of ​​520m 2 / kg, and obtain gelling material A.

[0046] 3. Performance Testing: Cementitious Material A was comprehensively tested for its performance. The three-day compressive strength test result was 15 MPa. Loading to failure was performed using a pressure testing machine, and the failure load was recorded and calculated. The 28-day compressive strength reached 35 MPa. Standard curing conditions were used, and testing was conducted after the curing age. Impermeability testing was conducted using a step-by-step pressurization method, and the results showed that the impermeability grade reached P6.

[0047] Example 3

[0048] This embodiment provides a sulfonated mud-based cementitious material.

[0049] 1. Raw material formula: 40 parts of sulfonated mud, 20 parts of slag, 20 parts of fly ash, 6 parts of gypsum, and 7 parts of sodium silicate.

[0050] 2. Preparation process: sulfonated slurry is dehydrated to a water content of 25%, slag and fly ash are ground to a specific surface area of ​​450m 2 / kg. When mixing, the mixer speed is 110r / min and the stirring time is 18 minutes. The temperature of the aging bin is controlled at 28℃ and the humidity is controlled at 65%. The final powder is ground to a specific surface area of ​​550m 2 / kg, and obtain gelling material B.

[0051] 3. Performance Test: The 3-day compressive strength of cementitious material B is 18MPa, and the 28-day compressive strength is 40MPa. The results of the impermeability test show that its impermeability grade reaches P7.

[0052] Example 4

[0053] This embodiment provides a sulfonated mud-based cementitious material.

[0054] 1. Raw material formula: 50 parts of sulfonated mud, 30 parts of slag, 20 parts of fly ash, 10 parts of gypsum, and 8 parts of alkaline activator.

[0055] 2. Preparation process: Referring to the preparation methods of Examples 2 and 3, the sulfonated slurry is dehydrated, the slag and fly ash are ground, and the materials are mixed, stirred, aged and finally ground to obtain a cementitious material D.

[0056] 3. Performance test: The 3-day compressive strength and 28-day compressive strength of cementitious material D are lower than those of cementitious material B. The results of the impermeability test show that its impermeability grade is also lower than that of cementitious material B. Sulfonated mud itself has good high temperature resistance and corrosion resistance, and can maintain stability under specific conditions. These characteristics give it certain advantages when used as a cementitious material. The proportion of the sulfonated mud component in cementitious material B reaches a performance balance in the cementitious material. At this ratio, the high temperature resistance, corrosion resistance and other possible performance characteristics of the sulfonated mud are best exerted, thereby improving the performance of the entire cementitious material. Too little sulfonated mud (such as 30 parts) may not fully exert its performance advantages; too much sulfonated mud (such as 50 parts) may inhibit its performance advantages. Therefore, 40 parts is an optimal ratio that can both exert the performance advantages of sulfonated mud and avoid side effects.

[0057] Comparative Example

[0058] The difference between the comparative example and Examples 2, 3 and 4 is that the comparative example adopts a traditional cement formula to prepare cement, wherein no sulfonated mud is added.

[0059] 1. Raw material formula: adopt traditional cement formula, the main raw materials are limestone, clay, gypsum, etc., without adding sulfonated mud.

[0060] 2. Preparation process: According to the traditional cement production process, cement C is obtained through the steps of raw material preparation, clinker calcination, cement grinding, etc.

[0061] 3. Performance comparison: Compare the performance of cementitious materials A, B, and D with that of cement C. In terms of compressive strength, the early strength of cementitious materials A and B is slightly lower than that of cement C, but the 28-day strength is comparable. In terms of impermeability, the impermeability grades of cementitious materials A and B are higher than that of cement C. In terms of environmental protection, cement C emits huge amounts of carbon dioxide during its production process, while cementitious materials A, B, and D achieve resource utilization of sulfonated mud with almost zero emissions. In terms of cost, the production cost of cementitious materials A, B, and D is approximately 40 yuan / ton lower than that of cement C. Comprehensively comparing, cementitious materials A, B, and D have obvious advantages in terms of environmental protection and cost, and their performance can meet the needs of most construction projects.

[0062] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations of the present invention are possible. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. A sulfonated mud-based cementitious material, characterized in that: The composition comprises the following components in parts by weight: 30-50 parts of sulfonated mud, 20-30 parts of active auxiliary materials, 10-20 parts of fly ash, and 3-8 parts of active activator.

2. The sulfonated mud-based cementitious material according to claim 1, characterized in that: The active auxiliary materials include: one or more of slag, cement, silica fume, carbide slag, steel slag, red mud and biochar-based materials.

3. The sulfonated mud-based cementitious material according to claim 1, characterized in that: The active stimulant includes one or more of alkaline stimulants, acidic stimulants, salt stimulants and biological agents, wherein multiple components constitute a composite stimulant.

4. The sulfonated mud-based cementitious material according to claim 3, characterized in that: The alkaline activator includes one or more of sodium hydroxide, potassium hydroxide and sodium silicate.

5. The sulfonated mud-based cementitious material according to any one of claims 1 to 4, characterized in that: The sulfonated mud-based cementitious material includes: 5-10 parts of gypsum or lime.

6. A method for preparing a sulfonated slurry-based gelling material according to any one of claims 1 to 5, characterized in that: The following steps are involved: S1. Raw material pretreatment: dehydration of sulfonated slurry to control moisture content, grinding of active ingredients and fly ash; S2 mixing: The active material, fly ash, active activator and dehydrated sulfonated slurry are stirred and mixed uniformly in a mass ratio; S3. Aging treatment: Aging the uniformly mixed material to obtain a preliminary gel material.

7. The method for preparing a sulfonated slurry-based gelling material according to claim 6, characterized in that: In the dehydration treatment of the sulfonated mud to control the water content in step S1, the sulfonated mud is pre-screened and impurities are removed, and the sulfonated mud is dehydrated to a water content of less than 30%.

8. The method for preparing a sulfonated slurry-based gelling material according to claim 6, characterized in that: In the grinding process of the active auxiliary materials and fly ash in step S1, the specific surface area of ​​the grinding process material is 400-500m 2 / kg; and / or In step S4, the specific surface area of ​​the grinding material is 500-600m 2 / kg.

9. The method for preparing a sulfonated slurry-based gelling material according to claim 6, characterized in that: Step S2 is carried out in a mixer at a rotation speed of 80-120 r / min; and / or Gypsum or lime is added into the mixer according to the mass ratio and mixed with the materials.

10. The method for preparing a sulfonated slurry-based gelling material according to any one of claims 6 to 9, characterized in that: The preparation method of the sulfonated mud-based gelling material comprises the following steps: S4. Secondary grinding treatment: grinding the preliminary gel material to further increase the specific surface area of ​​the preliminary gel material to obtain a gel material product.

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