Preparation method of fast-hardening early-strength sulphoaluminate grouting material and grouting material thereof

Abstract

The present invention discloses a method for preparing a fast-hardening, early-strengthening sulphoaluminate grouting material and the grouting material. The preparation method comprises the following steps: S1, mixing vinyl pyrrolidone, N,N-dimethylacrylamide, and acrylate emulsion to obtain a preliminary mixed liquid; S2, adding sulphoaluminate clinker to the preliminary mixed liquid to obtain an intermediate mixed product; S3, adding fatty alcohol polyoxyethylene ether to the intermediate mixed product to obtain product A; S4, mixing water, phosphogypsum, and carbide slag to obtain an alkaline mixed product; S5, adding a regulator and a retarder to the alkaline mixed product to obtain product B; S6, mixing product A with product B to obtain the prepared fast-hardening, early-strengthening sulphoaluminate grouting material. The raw materials of the grouting material include sulphoaluminate clinker, vinyl pyrrolidone, N,N-dimethylacrylamide, acrylate emulsion, fatty alcohol polyoxyethylene ether, water, phosphogypsum, carbide slag, a regulator, and a retarder.

Description

Technical Field

[0001] The invention relates to the field of cement, in particular to a preparation method of a fast-hardening and early-strengthening sulphoaluminate grouting material and the grouting material. Background Art

[0002] Grouting technology is indispensable in deep-ground technology systems. Grouting refers to the use of physical or chemical methods to inject solidifiable liquid materials into cracks in the injected matrix, thereby improving its physical and mechanical properties. Grouting is widely used in underground engineering fields such as safe mining and tunnel water blocking due to its good economic efficiency. The key to grouting lies in the performance of the grouting material. At present, the grouting materials used in underground engineering are mainly chemical slurries and silicate cement-based grouting materials. Chemical slurries have the advantages of good permeability and fast coagulation and hardening, but they are expensive and generally toxic and easily harmful to the environment, and their application is gradually restricted. Silicate cement-based grouting materials have the characteristics of wide material sources, low cost, and non-toxicity, but are limited by the hydration characteristics of their constituent minerals, and generally have defects such as long coagulation time, low early strength, low stone rate, and easy shrinkage. It can be seen that the performance of existing grouting materials cannot fully meet the needs of underground engineering.

[0003] In order to promote the green, healthy and high-quality development of underground engineering and meet the actual needs of various grouting projects, in recent years, research on the use of sulphoaluminate grouting materials to prepare new cement-based grouting materials (sulphoaluminate grouting material-based grouting materials, abbreviated as SCBGM) has gradually emerged at home and abroad. Sulphoaluminate grouting material is a special cement independently developed by the China Building Materials Research Institute in the 1970s. Unlike silicate cement, the clinker of sulphoaluminate grouting material contains a large amount of anhydrous calcium sulphoaluminate minerals, and the energy consumption during the firing process is low and the carbon dioxide emissions are relatively low. Therefore, sulphoaluminate grouting material can be regarded as a green, low-carbon and environmentally friendly cementitious material. During the hydration process of sulphoaluminate grouting material, the anhydrous calcium sulphoaluminate minerals contained in its clinker will be rapidly converted into hydration products such as ettringite and aluminum gel, thereby significantly giving it excellent properties such as fast setting and hardening, early strength and high strength, high impermeability, high frost resistance and corrosion resistance.

[0004] Gypsum and lime are key components in the production of SCBGM. Gypsum provides the sulfate ions necessary for the conversion of anhydrous calcium sulfoaluminate minerals in the clinker of sulfoaluminate grouting materials into ettringite. Lime effectively increases the alkalinity of the slurry, significantly accelerating the formation of ettringite and enabling the slurry to rapidly set and harden, developing strength. However, with the continued strengthening of environmental protection in my country and the implementation of large-scale restrictions on mining and burning in the building materials industry, the availability of natural gypsum and lime has become severely limited. Therefore, it is necessary to explore new materials for the production of SCBGM to expand its development path. Summary of the Invention

[0005] The purpose of the present invention is to solve the above problems and provide a method for preparing a fast-hardening and early-strengthening sulphoaluminate grouting material which is simple to operate and cost-effective and a grouting material thereof.

[0006] In order to achieve the above object, the technical solution of the present invention is:

[0007] A method for preparing a fast-hardening and early-strengthening sulphoaluminate grouting material comprises the following steps:

[0008] S1. Evenly mix vinyl pyrrolidone and N,N-dimethylacrylamide, and slowly add acrylate emulsion, stirring at a speed of 50 to 80 r / min while adding the acrylate emulsion to obtain a preliminary mixed liquid;

[0009] S2. After heating the preliminary mixed liquid to 60-80° C., adding sulphoaluminate clinker, stirring it at a speed of 150-300 r / min for 20-40 minutes, and cooling it to room temperature to obtain an intermediate mixed product;

[0010] S3, adding fatty alcohol polyoxyethylene ether to the intermediate mixed product, stirring evenly and then standing for 2 to 3 hours to obtain product A;

[0011] S4, mixing water, phosphogypsum, and carbide slag, heating to 100-120° C. and stirring at a speed of 100-200 r / min for 2-3 hours, and cooling to room temperature to obtain an alkaline mixed product;

[0012] S5. Add a regulator and a retarder to the alkaline mixed product in sequence and stir evenly. Let it stand for 1 to 2 hours to obtain product B;

[0013] S6. Mix product A and product B, and stir them evenly to obtain the prepared fast-hardening and early-strengthening sulphoaluminate grouting material.

[0014] A grouting material, the raw materials of which include sulphoaluminate clinker, vinyl pyrrolidone, N,N-dimethylacrylamide, acrylate emulsion, fatty alcohol polyoxyethylene ether, water, phosphogypsum, carbide slag, a regulator, and a retarder; the weight proportions of the raw materials are as follows: 8-12 parts of sulphoaluminate clinker, 2-4 parts of vinyl pyrrolidone, 1-3 parts of N,N-dimethylacrylamide, 3-5 parts of acrylate emulsion, 1-3 parts of fatty alcohol polyoxyethylene ether, 15-18 parts of water, 10-13 parts of phosphogypsum, 5-8 parts of carbide slag, 2-4 parts of regulator, and 1-3 parts of retarder.

[0015] Furthermore, in the grouting material, the weight proportions of each raw material component are: 10 parts of sulfoaluminate clinker, 3 parts of vinyl pyrrolidone, 2 parts of N,N-dimethylacrylamide, 4 parts of acrylic emulsion, 2 parts of fatty alcohol polyoxyethylene ether, 16 parts of water, 12 parts of phosphogypsum, 6 parts of carbide slag, 3 parts of regulator, and 2 parts of retarder.

[0016] Furthermore, the sulphoaluminate clinker is made by uniformly mixing bauxite powder, lithium slag powder, calcium aluminate powder and perovskite powder and then calcining them at high temperature; the weight proportions of the bauxite powder, lithium slag powder, calcium aluminate powder and perovskite powder are 7 to 10 parts of bauxite powder, 2 to 3 parts of lithium slag powder, 3 to 4 parts of calcium aluminate powder and 1 to 2 parts of perovskite powder respectively.

[0017] Furthermore, the regulator is a mixture of one or more of cross-linked polyacrylic acid salt, sodium ethylenediaminetetramethylenephosphonate, and dioctadecyldimethylammonium chloride.

[0018] Furthermore, the retarder is one of tetrahydroxyethylethylenediamine and sodium lignin sulfonate, or a mixture of the two.

[0019] Compared with the prior art, the present invention has the following advantages and positive effects:

[0020] The present invention uses phosphogypsum to replace natural gypsum and carbide slag to replace natural lime, and generates sulphoaluminate grouting material slurry by reacting phosphogypsum, carbide slag and sulphoaluminate clinker, which effectively realizes the raw material replacement of natural gypsum and natural lime in the production process of sulphoaluminate grouting material slurry, and opens a new path for the development of SCBGM; on the other hand, the components in the carbide slag can eliminate the adverse effects of soluble P and F impurities in phosphogypsum on the performance of SCBGM, and the synergistic production effect of phosphogypsum and carbide slag effectively improves the production quality of SCBGM; and, in addition, phosphogypsum is a by-product generated in the production process of wet-process phosphoric acid, and its main component is calcium sulfate dihydrate. Random storage will cause pollution to the environment. The present invention effectively solves the storage and treatment problems of phosphogypsum by using phosphogypsum and carbide slag in combination, realizes waste utilization, and reduces the production cost of SCBGM, making a certain contribution to the recycling of chemical resources. DETAILED DESCRIPTION

[0021] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions 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, any modifications, equivalent replacements, improvements, etc., shall be included in the scope of protection of the present invention.

[0022] Example 1. This example discloses a fast-hardening and early-strengthening sulphoaluminate grouting material, whose raw materials include sulphoaluminate clinker, vinyl pyrrolidone, N,N-dimethylacrylamide, acrylate emulsion, fatty alcohol polyoxyethylene ether, water, phosphogypsum, carbide slag, cross-linked polyacrylic acid salt, and tetrahydroxyethylethylenediamine; the weight proportions of each raw material component are: 8 parts of sulphoaluminate clinker, 2 parts of vinyl pyrrolidone, 1 part of N,N-dimethylacrylamide, 3 parts of acrylate emulsion, 1 part of fatty alcohol polyoxyethylene ether, 15 parts of water, 10 parts of phosphogypsum, 5 parts of carbide slag, 2 parts of cross-linked polyacrylic acid salt, and 1 part of tetrahydroxyethylethylenediamine.

[0023] The sulphoaluminate clinker is made by uniformly mixing bauxite powder, lithium slag powder, calcium aluminate powder and perovskite powder and then calcining them at high temperature; the weight proportions of the bauxite powder, lithium slag powder, calcium aluminate powder and perovskite powder are 7 parts of bauxite powder, 2 parts of lithium slag powder, 3 parts of calcium aluminate powder and 1 part of perovskite powder respectively.

[0024] At the same time, this embodiment discloses a method for preparing the above-mentioned fast-hardening and early-strengthening sulphoaluminate grouting material, which comprises the following steps:

[0025] S1. Evenly mix vinyl pyrrolidone and N,N-dimethylacrylamide, and slowly add acrylate emulsion, stirring at a speed of 50 r / min while adding the acrylate emulsion to obtain a preliminary mixed liquid;

[0026] S2. After heating the preliminary mixed liquid to 60° C., the sulphoaluminate clinker was added, and the mixture was stirred at a speed of 150 r / min for 20 minutes. After cooling to room temperature, an intermediate mixed product was obtained;

[0027] S3, adding fatty alcohol polyoxyethylene ether to the intermediate mixed product, stirring evenly and then standing for 2 hours to obtain product A;

[0028] S4, mixing water, phosphogypsum, and carbide slag, heating to 100° C. and stirring at a speed of 100 r / min for 2 hours, and cooling to room temperature to obtain an alkaline mixed product;

[0029] S5. Add cross-linked polyacrylate and tetrahydroxyethylethylenediamine to the alkaline mixed product in sequence and stir evenly. Let stand for 1 hour to obtain product B;

[0030] S6. Mix product A and product B, and stir them evenly to obtain the prepared fast-hardening and early-strengthening sulphoaluminate grouting material.

[0031] Example 2. This example discloses a fast-hardening and early-strengthening sulphoaluminate grouting material, whose raw materials include sulphoaluminate clinker, vinyl pyrrolidone, N,N-dimethylacrylamide, acrylate emulsion, fatty alcohol polyoxyethylene ether, water, phosphogypsum, carbide slag, sodium ethylenediaminetetramethylenephosphonate, and sodium lignin sulfonate; the weight proportions of each raw material component are: 10 parts of sulphoaluminate clinker, 3 parts of vinyl pyrrolidone, 2 parts of N,N-dimethylacrylamide, 4 parts of acrylate emulsion, 2 parts of fatty alcohol polyoxyethylene ether, 16 parts of water, 12 parts of phosphogypsum, 6 parts of carbide slag, 3 parts of sodium ethylenediaminetetramethylenephosphonate, and 2 parts of sodium lignin sulfonate.

[0032] The sulphoaluminate clinker is made by uniformly mixing bauxite powder, lithium slag powder, calcium aluminate powder and perovskite powder and then calcining them at high temperature; the weight proportions of the bauxite powder, lithium slag powder, calcium aluminate powder and perovskite powder are 8 parts of bauxite powder, 2 parts of lithium slag powder, 4 parts of calcium aluminate powder and 2 parts of perovskite powder respectively.

[0033] At the same time, this embodiment discloses a method for preparing the above-mentioned fast-hardening and early-strengthening sulphoaluminate grouting material, which comprises the following steps:

[0034] S1. Evenly mix vinyl pyrrolidone and N,N-dimethylacrylamide, and slowly add acrylate emulsion, stirring at a speed of 60 r / min while adding the acrylate emulsion to obtain a preliminary mixed liquid;

[0035] S2. After heating the preliminary mixed liquid to 70° C., adding sulphoaluminate clinker, stirring at a speed of 200 r / min for 30 minutes, and cooling to room temperature to obtain an intermediate mixed product;

[0036] S3, adding fatty alcohol polyoxyethylene ether to the intermediate mixed product, stirring evenly and then standing for 2 hours to obtain product A;

[0037] S4, mixing water, phosphogypsum, and carbide slag, heating to 110° C. and stirring at a speed of 150 r / min for 3 hours, and cooling to room temperature to obtain an alkaline mixed product;

[0038] S5. Sodium ethylenediaminetetramethylenephosphonate and sodium ligninsulfonate are sequentially added to the alkaline mixed product and stirred evenly. The mixture is allowed to stand for 2 hours to obtain product B.

[0039] S6. Mix product A and product B, and stir them evenly to obtain the prepared fast-hardening and early-strengthening sulphoaluminate grouting material.

[0040] Example 3. This example discloses a fast-hardening and early-strengthening sulphoaluminate grouting material, whose raw materials include sulphoaluminate clinker, vinyl pyrrolidone, N,N-dimethylacrylamide, acrylate emulsion, fatty alcohol polyoxyethylene ether, water, phosphogypsum, carbide slag, dioctadecyl dimethyl ammonium chloride, a mixture of tetrahydroxyethylethylenediamine and sodium lignin sulfonate; the weight proportions of each raw material component are: 12 parts of sulphoaluminate clinker, 4 parts of vinyl pyrrolidone, 3 parts of N,N-dimethylacrylamide, 5 parts of acrylate emulsion, 3 parts of fatty alcohol polyoxyethylene ether, 18 parts of water, 13 parts of phosphogypsum, 8 parts of carbide slag, 4 parts of dioctadecyl dimethyl ammonium chloride, and 3 parts of a mixture of tetrahydroxyethylethylenediamine and sodium lignin sulfonate.

[0041] The sulphoaluminate clinker is prepared by uniformly mixing bauxite powder, lithium slag powder, calcium aluminate powder and perovskite powder and then calcining them at high temperature; the weight proportions of the bauxite powder, lithium slag powder, calcium aluminate powder and perovskite powder are 10 parts of bauxite powder, 3 parts of lithium slag powder, 4 parts of calcium aluminate powder and 2 parts of perovskite powder respectively.

[0042] At the same time, this embodiment discloses a method for preparing the above-mentioned fast-hardening and early-strengthening sulphoaluminate grouting material, which comprises the following steps:

[0043] S1. Evenly mix vinyl pyrrolidone and N,N-dimethylacrylamide, and slowly add acrylate emulsion, stirring at a speed of 80 r / min while adding the acrylate emulsion to obtain a preliminary mixed liquid;

[0044] S2. After heating the preliminary mixed liquid to 80° C., adding sulphoaluminate clinker, stirring at a speed of 300 r / min for 40 minutes, and cooling to room temperature to obtain an intermediate mixed product;

[0045] S3, adding fatty alcohol polyoxyethylene ether to the intermediate mixed product, stirring evenly and then standing for 3 hours to obtain product A;

[0046] S4, mixing water, phosphogypsum, and carbide slag, heating to 120° C. and stirring at a speed of 200 r / min for 3 hours, and cooling to room temperature to obtain an alkaline mixed product;

[0047] S5. Add dioctadecyldimethylammonium chloride and a mixture of tetrahydroxyethylethylenediamine and sodium lignin sulfonate to the alkaline mixed product in sequence and stir evenly. Let stand for 2 hours to obtain product B;

[0048] S6. Mix product A and product B, and stir them evenly to obtain the prepared fast-hardening and early-strengthening sulphoaluminate grouting material.

[0049] In the process of producing the SCBGM system, ettringite is produced. The formation process of ettringite can be described as follows: first, the aluminate ions AlO2 released by the dissolution of the sulphoaluminate clinker particles are - Combined with two OH - ion and 2 H2O molecules to form [Al(OH)6] 3- Alumina octahedron, followed by [Al(OH)6] 3- Alumina octahedron and Ca 2+ Combines with H2O to form {Ca6[Al(OH)6]224H2O} 6+ Polyhedral cylinder, the last 3 SO4 2- and 2 H2O molecules into {Ca6[Al(OH)6]224H2O} 6+ A complete ettringite crystal structure is formed in the grooves of the polyhedral columns, which gives the solidified sulphoaluminate grouting material a stable structural strength.

[0050] At the same time, the ettringite crystals formed in the alkalinity environment provided by carbide slag show a fine needle-like morphology, which gives the SCBGM hardened body the characteristics of micro-expansion and has a good grouting solidification effect.

[0051] Based on the hydration characteristics of SCBGM, the present invention prepares it into a two-liquid type (i.e., two products A and B) to prevent its slurry from solidifying too quickly and thus affecting construction operations. Mixing them evenly before use allows the fast-hardening and early-strengthening sulphoaluminate grouting material slurry to quickly achieve a solidification effect in a short time.

[0052] The comprehensive content of phosphogypsum and carbide slag in the SCBGM developed in the present invention reaches 50% or more, which effectively realizes the large-scale and resource-based utilization of phosphogypsum and carbide slag; at the same time, after testing and analysis, the SCBGM slurry developed in the present invention has good stability (1h water bleeding rate ≤5%), the setting time can be accurately adjusted within 30min, and the 2h early compressive strength can reach more than 15MPa, which can fully meet the construction and use needs of the construction industry and the underground engineering field, and has made certain contributions to the development and construction of underground engineering.

[0053] The present invention uses phosphogypsum to replace natural gypsum and carbide slag to replace natural lime, and generates sulphoaluminate grouting material slurry by reacting phosphogypsum, carbide slag and sulphoaluminate clinker, which effectively realizes the raw material replacement of natural gypsum and natural lime in the production process of sulphoaluminate grouting material slurry, and opens a new path for the development of SCBGM; on the other hand, the components in the carbide slag can eliminate the adverse effects of soluble P and F impurities in phosphogypsum on the performance of SCBGM, and the synergistic production effect of phosphogypsum and carbide slag effectively improves the production quality of SCBGM; and, in addition, phosphogypsum is a by-product generated in the production process of wet-process phosphoric acid, and its main component is calcium sulfate dihydrate. Random storage will cause pollution to the environment. The present invention effectively solves the storage and treatment problems of phosphogypsum by using phosphogypsum and carbide slag in combination, realizes waste utilization, and reduces the production cost of SCBGM, making a certain contribution to the recycling of chemical resources.

Claims

1. A method for preparing a fast-hardening and early-strength sulphoaluminate grouting material, characterized by: The following steps are involved: S1. Evenly mix vinyl pyrrolidone and N,N-dimethylacrylamide, and slowly add acrylate emulsion, stirring at a speed of 50 to 80 r / min while adding the acrylate emulsion to obtain a preliminary mixed liquid; S2. After heating the preliminary mixed liquid to 60-80° C., adding sulphoaluminate clinker, stirring it at a speed of 150-300 r / min for 20-40 minutes, and cooling it to room temperature to obtain an intermediate mixed product; S3, adding fatty alcohol polyoxyethylene ether to the intermediate mixed product, stirring evenly and then standing for 2 to 3 hours to obtain product A; S4, mixing water, phosphogypsum, and carbide slag, heating to 100-120° C. and stirring at a speed of 100-200 r / min for 2-3 hours, and cooling to room temperature to obtain an alkaline mixed product; S5. Add a regulator and a retarder to the alkaline mixed product in sequence and stir evenly. Let it stand for 1 to 2 hours to obtain product B; S6. Mixing product A and product B, and stirring evenly to obtain the prepared fast-hardening and early-strengthening sulphoaluminate grouting material; The weight proportions of the raw materials in the rapid-hardening and early-strengthening sulphoaluminate grouting material are as follows: 8-12 parts of sulphoaluminate clinker, 2-4 parts of vinyl pyrrolidone, 1-3 parts of N,N-dimethylacrylamide, 3-5 parts of acrylate emulsion, 1-3 parts of fatty alcohol polyoxyethylene ether, 15-18 parts of water, 10-13 parts of phosphogypsum, 5-8 parts of carbide slag, 2-4 parts of regulator, and 1-3 parts of retarder. The regulator is a mixture of one or more of cross-linked polyacrylic acid salt, sodium ethylenediamine tetramethylenephosphonate, and dioctadecyl dimethyl ammonium chloride; the retarder is a mixture of one or two of tetrahydroxyethylethylenediamine and sodium lignin sulfonate; The 2h early compressive strength of the fast-hardening and early-strength sulphoaluminate grouting material is above 15 MPa.

2. A grouting material prepared by the preparation method of the fast-hardening and early-strength sulphoaluminate grouting material according to claim 1.

3. The grouting material according to claim 2, wherein: In the grouting material, the weight parts of each raw material component are: 10 parts of sulphoaluminate clinker, 3 parts of vinyl pyrrolidone, 2 parts of N,N-dimethylacrylamide, 4 parts of acrylic emulsion, 2 parts of fatty alcohol polyoxyethylene ether, 16 parts of water, 12 parts of phosphogypsum, 6 parts of calcium carbide slag, 3 parts of regulator, and 2 parts of retarder.

4. The grouting material according to claim 3, wherein: The sulphoaluminate clinker is prepared by uniformly mixing bauxite powder, lithium slag powder, calcium aluminate powder and perovskite powder and then calcining them at high temperature; the weight proportions of the bauxite powder, lithium slag powder, calcium aluminate powder and perovskite powder are 7 to 10 parts of bauxite powder, 2 to 3 parts of lithium slag powder, 3 to 4 parts of calcium aluminate powder and 1 to 2 parts of perovskite powder respectively.