Graphite oxide alkali-free liquid accelerator and preparation method thereof
By preparing an alkali-free liquid accelerator using graphite oxide, and by adding an ion regulator to the graphite oxide dispersion and the alkali-free accelerator, the problems of poor compatibility and insufficient stability of the alkali-free liquid accelerator with cement were solved, achieving low-cost, high-stability, and high-strength concrete.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- YUNCHENG UNIVERSITY
- Filing Date
- 2023-07-14
- Publication Date
- 2026-04-17
AI Technical Summary
Existing alkali-free liquid quick-setting agents have poor compatibility with cement, low stability, and are prone to sedimentation after prolonged storage, and are also costly.
Using graphite oxide dispersion and alkali-free quick-setting agent as the main raw materials, alkali-free liquid quick-setting agent of graphite oxide is prepared through a specific process. Ion regulators are added to control the reaction rate and stability. The preparation process includes preparing graphite oxide dispersion and activating alkali-free quick-setting agent, and finally homogenization and aging treatment.
The prepared alkali-free liquid accelerator of graphite oxide has a pH value of 2.8-3.8, low cost, small dosage, long stability time, and can improve concrete strength. It solves the problem of poor applicability of alkali-free liquid accelerators with cement and has better stability.
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Figure CN116813233B_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of building materials, specifically to an alkali-free liquid quick-setting agent for graphite oxide and its preparation method. Background Technology
[0002] Accelerators are concrete setting accelerators that speed up the setting and hardening of concrete. They are indispensable admixtures in major engineering projects such as tunnel spraying, railways, and bridges. The development of accelerators has evolved from powder accelerators to liquid accelerators, and from alkali-based accelerators to liquid accelerators. While powder accelerators offer good setting acceleration and are inexpensive, they suffer from severe dust generation during construction and require sophisticated equipment. Alkali-based accelerators have high alkali content, leading to significant strength loss in the later stages of concrete formation and strong corrosiveness. The emergence of liquid accelerators has solved the problem of severe dust generation associated with powder accelerators, while alkali-free accelerators have addressed the issues of high alkali content, significant strength loss in the later stages, and strong corrosiveness associated with alkali-based accelerators. Furthermore, alkali-free liquid accelerators offer advantages such as safety and environmental friendliness, no strength loss, and no alkali-aggregate reaction.
[0003] With the increase in the types of admixtures and the decrease in high-quality building raw materials, issues have arisen regarding the applicability of alkali-free liquid accelerators to cement and the gradually increasing application costs. In particular, the implementation of the new national concrete standard has brought unprecedented challenges to the preparation of various admixtures, especially alkali-free liquid accelerators. Summary of the Invention
[0004] To address one of the aforementioned technical deficiencies, this application provides an alkali-free liquid quick-setting agent for graphite oxide and its preparation method.
[0005] According to a first aspect of the embodiments of this application, an alkali-free liquid quick-setting agent for graphite oxide is provided, comprising the following raw materials in parts by weight: 100 parts of alkali-free quick-setting agent and 1-10 parts of graphite oxide dispersion.
[0006] Preferably, the alkali-free liquid quick-setting agent for graphite oxide further includes 0.1-1 parts by weight of an ion regulator.
[0007] More preferably, the ion regulator comprises the following raw materials in parts by weight: 25-40 parts of polyaluminum chloride, 20-30 parts of triethanolamine, 5-10 parts of lactic acid, and 30-50 parts of deionized water.
[0008] Preferably, the alkali-free quick-setting agent comprises the following raw materials in parts by weight: 45-60 parts of polyaluminum sulfate, 10-30 parts of aluminum chloride, 3-15 parts of amine reinforcing component, 1-5 parts of nano silica, 1-3 parts of strong adsorption component, and 3-10 parts of acidity regulator.
[0009] More preferably, the strong adsorption component comprises the following raw materials in parts by weight: 25-45 parts maleic anhydride, 30-50 parts sodium methacrylate sulfonate, 30-45 parts 2-acrylamide-2-methylpropanesulfonic acid, and 2-5 parts lactic acid.
[0010] Preferably, the graphite oxide dispersion comprises the following raw materials in parts by weight: 20-30 parts concentrated sulfuric acid, 1-3 parts natural graphite, 1-3 parts sodium nitrate, 5-15 parts potassium permanganate, 2-10 parts hydrogen peroxide, 3-10 parts 5% hydrochloric acid, and 40-70 parts deionized water.
[0011] According to a second aspect of the embodiments of this application, a method for preparing an alkali-free liquid quick-setting agent for graphite oxide is provided, comprising the following steps:
[0012] S10, to prepare an oxide graphite dispersion;
[0013] S101. Pour concentrated sulfuric acid into a beaker, then place the beaker in an ice water bath, and slowly add natural graphite, sodium nitrate and potassium permanganate in sequence, stirring for 40 minutes.
[0014] S102, transfer the beaker to an oil bath at 37°C and stir for 30 minutes. After the temperature rises to 70-90°C, stir for another 30 minutes.
[0015] S103, then add hydrogen peroxide to the beaker until no more bubbles are produced to obtain a mixed solution, and the color of the mixed solution is bright yellow;
[0016] S104, the mixed solution is centrifuged to obtain a precipitate, the precipitate is first washed with 5% hydrochloric acid, and then washed with deionized water to obtain graphite oxide;
[0017] S105, dissolve graphite oxide in distilled water and disperse by ultrasonication to obtain a uniform graphite oxide dispersion.
[0018] S20, activated alkali-free quick-setting agent;
[0019] S30, Preparation of mixed solution: Add the prepared graphite oxide dispersion to the activated alkali-free quick-setting agent to obtain a mixed solution;
[0020] S40 is used to homogenize and age the mixed solution.
[0021] Stir the mixed solution for 1-2 hours, then stir for 3-5 hours to fully homogenize it; let it stand for 24 hours to age it, and you will get the alkali-free liquid quick-setting agent for graphite oxide.
[0022] Preferably, step S20, activating the alkali-free quick-setting agent, specifically includes:
[0023] S201, weigh out polyaluminum sulfate, aluminum chloride, amine reinforcing component, nano silica, strong adsorption component and acidity regulator;
[0024] S202 involves sequentially adding polyaluminum sulfate, aluminum chloride, amine-enhancing components, nano-silica, strong adsorption components, and acidity regulators into a reaction vessel and stirring for 1-3 hours to ensure uniform mixing, thereby obtaining an activated alkali-free quick-setting agent.
[0025] Preferably, step S20, activating the alkali-free quick-setting agent, specifically includes: weighing the alkali-free quick-setting agent and stirring for 1-3 hours to obtain the activated alkali-free quick-setting agent; in step S30, while adding the prepared graphite oxide dispersion to the activated alkali-free quick-setting agent, an ion regulator is added to obtain a mixed solution.
[0026] More preferably, the ion regulator comprises the following raw materials in parts by weight: 25-40 parts of polyaluminum chloride, 20-30 parts of triethanolamine, 5-10 parts of lactic acid, and 30-50 parts of deionized water.
[0027] An alkali-free liquid accelerator of graphite oxide was prepared using the alkali-free accelerator and graphite oxide dispersion provided in the embodiments of this application. The prepared alkali-free liquid accelerator of graphite oxide has a pH value of 2.8-3.8, and is low in cost, requires small dosage, and has a long stabilization time. It can also improve the strength of concrete prepared using this alkali-free liquid accelerator of graphite oxide. This solves the problem of poor applicability of alkali-free liquid accelerators to cement in the prior art, as well as the problem of sedimentation due to the low stability of the accelerator after prolonged storage. Attached Figure Description
[0028] The accompanying drawings, which are included to provide a further understanding of this application and form part of this application, illustrate exemplary embodiments of this application and are used to explain this application, but do not constitute an undue limitation of this application. In the drawings:
[0029] Figure 1 An electron microscope image of a black powder obtained by vacuum freeze-drying a graphite oxide dispersion in an alkali-free liquid quick-setting agent provided in this application embodiment. Detailed Implementation
[0030] To make the technical solutions and advantages of the embodiments of this application clearer, the exemplary embodiments of this application will be described in further detail below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of this application, and not an exhaustive list of all embodiments. It should be noted that, unless otherwise specified, the embodiments and features in the embodiments of this application can be combined with each other.
[0031] To address the aforementioned issues, this application provides an alkali-free liquid quick-setting agent for graphite oxide, comprising the following parts by weight of raw materials: 100 parts of alkali-free quick-setting agent and 1-10 parts of graphite oxide dispersion.
[0032] An alkali-free liquid accelerator of graphite oxide was prepared using the alkali-free accelerator and graphite oxide dispersion provided in the embodiments of this application. The prepared alkali-free liquid accelerator of graphite oxide has a pH value of 2.8-3.8, and is low in cost, requires small dosage, and has a long stabilization time. It can also improve the strength of concrete prepared using this alkali-free liquid accelerator of graphite oxide. This solves the problem of poor applicability of alkali-free liquid accelerators to cement in the prior art, as well as the problem of sedimentation due to the low stability of the accelerator after prolonged storage.
[0033] Furthermore, the alkali-free liquid quick-setting agent for graphite oxide also includes 0.1-1 parts by mass of an ion regulator.
[0034] Furthermore, the ion regulator comprises the following raw materials in parts by weight: 25-40 parts polyaluminum chloride, 20-30 parts triethanolamine, 5-10 parts lactic acid, and 30-50 parts deionized water.
[0035] In this application, when the alkali-free quick-setting agent is a directly weighed finished alkali-free quick-setting agent, an ion regulator needs to be added. The ion regulator can maintain the ion concentration, control the reaction rate between graphite oxide and the alkali-free quick-setting agent, and make the prepared alkali-free liquid quick-setting agent of graphite oxide more stable.
[0036] Furthermore, the alkali-free quick-setting agent comprises the following raw materials in parts by weight: 45-60 parts of polyaluminum sulfate, 10-30 parts of aluminum chloride, 3-15 parts of amine reinforcing component, 1-5 parts of nano silica, 1-3 parts of strong adsorption component, and 3-10 parts of acidity regulator.
[0037] In this application, an alkali-free quick-setting agent is prepared using polyaluminum sulfate, aluminum chloride, amine reinforcing components, nano-silica, strong adsorption components, and acidity regulators. The prepared alkali-free quick-setting agent can be used to accelerate the setting and hardening of concrete.
[0038] Furthermore, the strong adsorption component comprises the following raw materials in parts by weight: 25-45 parts maleic anhydride, 30-50 parts sodium methacrylate sulfonate, 30-45 parts 2-acrylamide-2-methylpropanesulfonic acid, and 2-5 parts lactic acid.
[0039] Furthermore, the graphite oxide dispersion comprises the following raw materials in parts by weight: 20-30 parts concentrated sulfuric acid, 1-3 parts natural graphite, 1-3 parts sodium nitrate, 5-15 parts potassium permanganate, 2-10 parts hydrogen peroxide, 3-10 parts 5% hydrochloric acid, and 40-70 parts deionized water. In this application, the graphite oxide dispersion is prepared using concentrated sulfuric acid, natural graphite, sodium nitrate, potassium permanganate, hydrogen peroxide, 5% hydrochloric acid, and deionized water. The acidity of the prepared graphite oxide dispersion is similar to that of the alkali-free quick-setting agent, making it more convenient to directly add to the alkali-free quick-setting agent.
[0040] In Examples 1 to 3 of this application, alkali-free quick-setting agents were prepared, while in Examples 4 to 6, the alkali-free quick-setting agents used were directly obtained finished products. The preparation methods of Examples 1 to 6 are described in detail below.
[0041] Example 1
[0042] A method for preparing an alkali-free liquid quick-setting agent for graphite oxide includes the following steps:
[0043] S10, to prepare an oxide graphite dispersion;
[0044] S101. Pour 20 parts of concentrated sulfuric acid into a beaker, then place the beaker in an ice water bath, and slowly add 1 part of natural graphite, 1 part of sodium nitrate and 5 parts of potassium permanganate in sequence, and stir for 40 minutes.
[0045] S102, transfer the beaker to an oil bath at 37°C and stir for 30 minutes. After the temperature rises to 70-90°C, stir for another 30 minutes.
[0046] S103, then add 2 parts of hydrogen peroxide to the beaker until no more bubbles are produced to obtain a mixed solution, and the color of the mixed solution is bright yellow;
[0047] S104, the mixed solution is centrifuged to obtain a precipitate. The precipitate is first washed with 3 parts of 5% hydrochloric acid, and then washed with 40 parts of deionized water to obtain graphite oxide.
[0048] S105, dissolve graphite oxide in distilled water and disperse by ultrasonication to obtain a uniform graphite oxide dispersion.
[0049] S20, activated alkali-free quick-setting agent;
[0050] S201, weigh out 45 parts of polyaluminum sulfate, 10 parts of aluminum chloride, 3 parts of amine reinforcing component, 1 part of nano silica, 1 part of strong adsorption component and 3 parts of acidity regulator.
[0051] Specifically, the strong adsorption components include 25 parts of maleic anhydride, 30 parts of sodium methacrylate sulfonate, 30 parts of 2-acrylamide-2-methylpropanesulfonic acid, and 2 parts of lactic acid.
[0052] S202: Polyaluminum sulfate, aluminum chloride, amine reinforcing component, nano silica, strong adsorption component and acidity regulator are added to the reaction vessel in sequence and stirred for 1-3 hours to make the mixture uniform, and then activated alkali-free quick-setting agent is obtained.
[0053] S30, Preparation of mixed solution: Add 1 part of the prepared graphite oxide dispersion to 100 parts of the activated alkali-free quick-setting agent to obtain a mixed solution;
[0054] S40 is used to homogenize and age the mixed solution.
[0055] Stir the mixed solution for 1-2 hours, then stir for 3-5 hours to fully homogenize it; let it stand for 24 hours to age it, and you will get the alkali-free liquid quick-setting agent for graphite oxide.
[0056] Specifically, the black powder obtained by vacuum freeze-drying a dispersion of graphite oxide. Figure 1 An electron microscope image of a black powder obtained by vacuum freeze-drying a graphite oxide dispersion in an alkali-free liquid quick-setting agent provided in this application embodiment.
[0057] Example 2
[0058] A method for preparing an alkali-free liquid quick-setting agent for graphite oxide includes the following steps:
[0059] S10, to prepare an oxide graphite dispersion;
[0060] S101. Pour 25 parts of concentrated sulfuric acid into a beaker, then place the beaker in an ice water bath, and slowly add 2 parts of natural graphite, 2 parts of sodium nitrate and 12 parts of potassium permanganate in sequence, and stir for 40 minutes.
[0061] S102, transfer the beaker to an oil bath at 37°C and stir for 30 minutes. After the temperature rises to 70-90°C, stir for another 30 minutes.
[0062] S103, then add 8 parts of hydrogen peroxide to the beaker until no more bubbles are produced to obtain a mixed solution, and the color of the mixed solution is bright yellow;
[0063] S104, the mixed solution is centrifuged to obtain a precipitate. The precipitate is first washed with 5 parts of 5% hydrochloric acid, and then washed with 50 parts of deionized water to obtain graphite oxide.
[0064] S105, dissolve graphite oxide in distilled water and disperse by ultrasonication to obtain a uniform graphite oxide dispersion.
[0065] S20, activated alkali-free quick-setting agent;
[0066] S201, weigh out 50 parts of polyaluminum sulfate, 20 parts of aluminum chloride, 10 parts of amine reinforcing component, 2 parts of nano silica, 2 parts of strong adsorption component and 8 parts of acidity regulator.
[0067] Specifically, the strong adsorption components include 35 parts maleic anhydride, 40 parts sodium methacrylate sulfonate, 40 parts 2-acrylamide-2-methylpropanesulfonic acid, and 3 parts lactic acid.
[0068] S202: Polyaluminum sulfate, aluminum chloride, amine reinforcing component, nano silica, strong adsorption component and acidity regulator are added to the reaction vessel in sequence and stirred for 1-3 hours to make the mixture uniform, and then activated alkali-free quick-setting agent is obtained.
[0069] S30, Preparation of mixed solution: Add 5 parts of the prepared graphite oxide dispersion to 100 parts of the activated alkali-free quick-setting agent to obtain a mixed solution;
[0070] S40 is used to homogenize and age the mixed solution.
[0071] Stir the mixed solution for 1-2 hours, then stir for 3-5 hours to fully homogenize it; let it stand for 24 hours to age it, and you will get the alkali-free liquid quick-setting agent for graphite oxide.
[0072] Example 3
[0073] A method for preparing an alkali-free liquid quick-setting agent for graphite oxide includes the following steps:
[0074] S10, to prepare an oxide graphite dispersion;
[0075] S101. Pour 30 parts of concentrated sulfuric acid into a beaker, then place the beaker in an ice water bath, and slowly add 3 parts of natural graphite, 3 parts of sodium nitrate and 15 parts of potassium permanganate in sequence, and stir for 40 minutes.
[0076] S102, transfer the beaker to an oil bath at 37°C and stir for 30 minutes. After the temperature rises to 70-90°C, stir for another 30 minutes.
[0077] S103, then add 10 parts of hydrogen peroxide to the beaker until no more bubbles are produced to obtain a mixed solution, and the color of the mixed solution is bright yellow;
[0078] S104, the mixed solution is centrifuged to obtain a precipitate, the precipitate is first washed with 10 parts of 5% hydrochloric acid, and then washed with 70 parts of deionized water to obtain graphite oxide.
[0079] S105, dissolve graphite oxide in distilled water and disperse by ultrasonication to obtain a uniform graphite oxide dispersion.
[0080] S20, activated alkali-free quick-setting agent;
[0081] S201, weigh out 60 parts of polyaluminum sulfate, 30 parts of aluminum chloride, 15 parts of amine reinforcing component, 5 parts of nano silica, 3 parts of strong adsorption component and 10 parts of acidity regulator.
[0082] Specifically, the strong adsorption components include 45 parts of maleic anhydride, 50 parts of sodium methacrylate sulfonate, 45 parts of 2-acrylamide-2-methylpropanesulfonic acid, and 5 parts of lactic acid.
[0083] S202: Polyaluminum sulfate, aluminum chloride, amine reinforcing component, nano silica, strong adsorption component and acidity regulator are added to the reaction vessel in sequence and stirred for 1-3 hours to make the mixture uniform, and then activated alkali-free quick-setting agent is obtained.
[0084] S30, Preparation of mixed solution: Add 10 parts of the prepared graphite oxide dispersion to 100 parts of the activated alkali-free quick-setting agent to obtain a mixed solution;
[0085] S40 is used to homogenize and age the mixed solution.
[0086] Stir the mixed solution for 1-2 hours, then stir for 3-5 hours to fully homogenize it; let it stand for 24 hours to age it, and you will get the alkali-free liquid quick-setting agent for graphite oxide.
[0087] Example 4
[0088] A method for preparing an alkali-free liquid quick-setting agent for graphite oxide includes the following steps:
[0089] S10, to prepare an oxide graphite dispersion;
[0090] S101. Pour 20 parts of concentrated sulfuric acid into a beaker, then place the beaker in an ice water bath, and slowly add 1 part of natural graphite, 1 part of sodium nitrate and 5 parts of potassium permanganate in sequence, and stir for 40 minutes.
[0091] S102, transfer the beaker to an oil bath at 37°C and stir for 30 minutes. After the temperature rises to 70-90°C, stir for another 30 minutes.
[0092] S103, then add 2 parts of hydrogen peroxide to the beaker until no more bubbles are produced to obtain a mixed solution, and the color of the mixed solution is bright yellow;
[0093] S104, the mixed solution is centrifuged to obtain a precipitate. The precipitate is first washed with 3 parts of 5% hydrochloric acid, and then washed with 40 parts of deionized water to obtain graphite oxide.
[0094] S105, dissolve graphite oxide in distilled water and disperse by ultrasonication to obtain a uniform graphite oxide dispersion.
[0095] S20, activated alkali-free quick-setting agent;
[0096] Weigh out the alkali-free quick-setting agent and stir for 1-3 hours to obtain the activated alkali-free quick-setting agent;
[0097] S30, Preparation of mixed solution: Add 1 part of the prepared graphite oxide dispersion and 0.1 part of the ion regulator to 100 parts of the activated alkali-free quick-setting agent to obtain a mixed solution;
[0098] Specifically, the ion regulator includes 25 parts of polyaluminum chloride, 20 parts of triethanolamine, 5 parts of lactic acid, and 30 parts of deionized water;
[0099] S40 is used to homogenize and age the mixed solution.
[0100] Stir the mixed solution for 1-2 hours, then stir for 3-5 hours to fully homogenize it; let it stand for 24 hours to age it, and you will get the alkali-free liquid quick-setting agent for graphite oxide.
[0101] Example 5
[0102] A method for preparing an alkali-free liquid quick-setting agent for graphite oxide includes the following steps:
[0103] S10, to prepare an oxide graphite dispersion;
[0104] S101. Pour 25 parts of concentrated sulfuric acid into a beaker, then place the beaker in an ice water bath, and slowly add 2 parts of natural graphite, 2 parts of sodium nitrate and 12 parts of potassium permanganate in sequence, and stir for 40 minutes.
[0105] S102, transfer the beaker to an oil bath at 37°C and stir for 30 minutes. After the temperature rises to 70-90°C, stir for another 30 minutes.
[0106] S103, then add 8 parts of hydrogen peroxide to the beaker until no more bubbles are produced to obtain a mixed solution, and the color of the mixed solution is bright yellow;
[0107] S104, the mixed solution is centrifuged to obtain a precipitate. The precipitate is first washed with 5 parts of 5% hydrochloric acid, and then washed with 50 parts of deionized water to obtain graphite oxide.
[0108] S105, dissolve graphite oxide in distilled water and disperse by ultrasonication to obtain a uniform graphite oxide dispersion.
[0109] S20, activated alkali-free quick-setting agent;
[0110] Weigh out the alkali-free quick-setting agent and stir for 1-3 hours to obtain the activated alkali-free quick-setting agent;
[0111] S30, Preparation of mixed solution: Add 5 parts of the prepared graphite oxide dispersion and 0.5 parts of ion regulator to 100 parts of the activated alkali-free quick-setting agent to obtain a mixed solution;
[0112] Specifically, the ion regulator includes 30 parts of polyaluminum chloride, 25 parts of triethanolamine, 8 parts of lactic acid, and 40 parts of deionized water;
[0113] S40 is used to homogenize and age the mixed solution.
[0114] Stir the mixed solution for 1-2 hours, then stir for 3-5 hours to fully homogenize it; let it stand for 24 hours to age it, and you will get the alkali-free liquid quick-setting agent for graphite oxide.
[0115] Example 6
[0116] A method for preparing an alkali-free liquid quick-setting agent for graphite oxide includes the following steps:
[0117] S10, to prepare an oxide graphite dispersion;
[0118] S101. Pour 30 parts of concentrated sulfuric acid into a beaker, then place the beaker in an ice water bath, and slowly add 3 parts of natural graphite, 3 parts of sodium nitrate and 15 parts of potassium permanganate in sequence, and stir for 40 minutes.
[0119] S102, transfer the beaker to an oil bath at 37°C and stir for 30 minutes. After the temperature rises to 70-90°C, stir for another 30 minutes.
[0120] S103, then add 10 parts of hydrogen peroxide to the beaker until no more bubbles are produced to obtain a mixed solution, and the color of the mixed solution is bright yellow;
[0121] S104, the mixed solution is centrifuged to obtain a precipitate, the precipitate is first washed with 10 parts of 5% hydrochloric acid, and then washed with 70 parts of deionized water to obtain graphite oxide.
[0122] S105, dissolve graphite oxide in distilled water and disperse by ultrasonication to obtain a uniform graphite oxide dispersion.
[0123] S20, activated alkali-free quick-setting agent;
[0124] Weigh out the alkali-free quick-setting agent and stir for 1-3 hours to obtain the activated alkali-free quick-setting agent;
[0125] S30, Preparation of mixed solution: Add 10 parts of the prepared graphite oxide dispersion and 1 part of the ion regulator to 100 parts of the activated alkali-free quick-setting agent to obtain a mixed solution;
[0126] Specifically, the ion regulator includes 40 parts of polyaluminum chloride, 30 parts of triethanolamine, 10 parts of lactic acid, and 50 parts of deionized water;
[0127] S40 is used to homogenize and age the mixed solution.
[0128] Stir the mixed solution for 1-2 hours, then stir for 3-5 hours to fully homogenize it; let it stand for 24 hours to age it, and you will get the alkali-free liquid quick-setting agent for graphite oxide.
[0129] The alkali-free quick-setting agent used in Examples 4 to 6 of this application is a finished alkali-free quick-setting agent with a stability time of one month. The stability time of the alkali-free liquid quick-setting agent for graphite oxide prepared using it can be increased to more than 3 months.
[0130] The preparation method of the alkali-free liquid accelerator for graphite oxide provided in this application is simple to operate. The prepared alkali-free liquid accelerator for graphite oxide has good applicability to cement and good stability. The acidity of the alkali-free accelerator is similar to that of the graphite oxide dispersion, eliminating the need for washing, drying, and re-dissolving with hydrochloric acid in the graphite oxide dispersion; it can be directly added to the alkali-free accelerator. Furthermore, since it includes the raw materials used in preparing the alkali-free liquid accelerator for graphite oxide, it can be considered to have the same beneficial effects as the product itself, which will not be elaborated further here.
[0131] Although preferred embodiments of this application have been described, those skilled in the art, upon learning the basic inventive concept, can make other changes and modifications to these embodiments. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments as well as all changes and modifications falling within the scope of this application.
[0132] Obviously, those skilled in the art can make various modifications and variations to this application without departing from the spirit and scope of this application. Therefore, if such modifications and variations fall within the scope of the claims of this application and their equivalents, this application also intends to include such modifications and variations.
Claims
1. A non-alkali liquid quick-setting agent for graphite oxide, characterized in that, The raw materials include the following parts by weight: 100 parts of alkali-free quick-setting agent, 1-10 parts of graphite oxide dispersion, and 0.1-1 parts of ion regulator; The ion regulator comprises the following raw materials in parts by weight: 25-40 parts polyaluminum chloride, 20-30 parts triethanolamine, 5-10 parts lactic acid, and 30-50 parts deionized water. The alkali-free quick-setting agent comprises the following raw materials in parts by weight: 45-60 parts of polyaluminum sulfate, 10-30 parts of aluminum chloride, 3-15 parts of amine reinforcing component, 1-5 parts of nano silica, 1-3 parts of strong adsorption component and 3-10 parts of acidity regulator. The strong adsorption component comprises the following raw materials in parts by weight: 25-45 parts maleic anhydride, 30-50 parts sodium methacrylate, 30-45 parts 2-acrylamide-2-methylpropanesulfonic acid, and 2-5 parts lactic acid. The graphite oxide dispersion is prepared using the following raw materials in parts by weight: 20-30 parts concentrated sulfuric acid, 1-3 parts natural graphite, 1-3 parts sodium nitrate, 5-15 parts potassium permanganate, 2-10 parts hydrogen peroxide, 3-10 parts 5% hydrochloric acid, and 40-70 parts deionized water.
2. The method for preparing an alkali-free liquid quick-setting agent for graphite oxide according to claim 1, characterized in that, Includes the following steps: S10, to prepare an oxide graphite dispersion; S101. Pour concentrated sulfuric acid into a beaker, then place the beaker in an ice water bath, and slowly add natural graphite, sodium nitrate and potassium permanganate in sequence, stirring for 40 minutes. S102, transfer the beaker to an oil bath at 37°C and stir for 30 minutes. After the temperature rises to 70~90°C, stir for another 30 minutes. S103, then add hydrogen peroxide to the beaker until no more bubbles are produced to obtain a mixed solution, and the color of the mixed solution is bright yellow; S104, the mixed solution is centrifuged to obtain a precipitate, the precipitate is first washed with 5% hydrochloric acid, and then washed with deionized water to obtain graphite oxide; S105, dissolve graphite oxide in distilled water and disperse by ultrasonication to obtain a uniform graphite oxide dispersion. S20, activated alkali-free quick-setting agent; Weigh out the alkali-free quick-setting agent and stir for 1-3 hours to activate it; S30, Preparation of mixed solution: Add the prepared graphite oxide dispersion to the activated alkali-free quick-setting agent to obtain a mixed solution; S40 is used to homogenize and age the mixed solution. Stir the mixed solution for 1-2 hours, then stir for 3-5 hours to fully homogenize it; let it stand for 24 hours to age it, and you will get the alkali-free liquid quick-setting agent for graphite oxide.
3. The method for preparing the alkali-free liquid quick-setting agent for graphite oxide according to claim 2, characterized in that, Step S20, activating the alkali-free quick-setting agent, specifically includes: S201, weigh out polyaluminum sulfate, aluminum chloride, amine reinforcing component, nano silica, strong adsorption component and acidity regulator; S202 involves sequentially adding polyaluminum sulfate, aluminum chloride, amine-enhancing components, nano-silica, strong adsorption components, and acidity regulators into a reaction vessel and stirring for 1-3 hours to ensure uniform mixing, thereby obtaining an activated alkali-free quick-setting agent.
4. The method for preparing the alkali-free liquid quick-setting agent for graphite oxide according to claim 2, characterized in that, Step S20, activating the alkali-free quick-setting agent, specifically includes: weighing the alkali-free quick-setting agent and stirring for 1-3 hours to obtain the activated alkali-free quick-setting agent; In step S30, an ion regulator is added to the prepared graphite oxide dispersion while the activated alkali-free quick-setting agent is added to obtain a mixed solution.
Citation Information
Patent Citations
Early strength type liquid alkali-free setting accelerator synthesized at normal temperature and preparation method of setting accelerator
CN108585587A