CN112745056B - Suspension type alkali-free liquid accelerator and preparation method thereof - Google Patents
Suspension type alkali-free liquid accelerator and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/10—Accelerators; Activators
- C04B2103/12—Set accelerators
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Abstract
The invention belongs to the technical field of concrete admixtures, and discloses a suspension type alkali-free liquid accelerator and a preparation method thereof. Firstly, respectively preparing magnesium-aluminum layered double hydroxide and an amino-terminated hyperbranched polymer, then adding the magnesium-aluminum layered double hydroxide and the amino-terminated hyperbranched polymer into water, uniformly stirring and dispersing, then adding aluminum sulfate and a pH regulator, and uniformly stirring and dispersing to obtain the suspension type alkali-free liquid accelerator. The magnesium-aluminum layered double hydroxides with high dispersibility and high specific surface area are further cooperated with the amino-terminated hyperbranched polymer to form an inorganic-organic polymer co-stabilization system and a tackifying system, so that a high-concentration supersaturated aluminum sulfate solution system can be suspended and stabilized, a good quick setting effect can be achieved, the early strength of the concrete can be improved, the rebound rate of the sprayed concrete can be reduced, and the pipe blockage phenomenon in the application process of the sprayed concrete can be effectively improved.
Description
Technical Field
The invention belongs to the technical field of concrete admixtures, and particularly relates to a suspension type alkali-free liquid accelerator and a preparation method thereof.
Background
The accelerator is a set control agent capable of accelerating the setting and hardening speed of concrete, and mainly has the functions of accelerating the hydration hardening of cement and forming enough strength in a short time so as to ensure the requirements of special construction. Conventional accelerators often include alkali metals, but these accelerators are strongly basic and often suffer from undesirable drawbacks, such as the presence of strong bases being likely to cause alkali-aggregate reactions that result in the destruction of the concrete structure and failure to fully meet construction engineering requirements. Meanwhile, the accelerator is too strong in alkalinity, poses certain threat to the health of constructors and has strong corrosive damage effect on the skin of a human body. Alkali-free accelerators are well known and evolving technologies for shotcrete applications. The chemistry of these accelerators is based on aluminium sulphate, in particular on a combination of aluminium salts such as aluminium sulphate, aluminium hydroxide and aluminium hydroxysulphate, which can be used in the form of a suspension.
Suspensions based on aluminium sulphate are generally unstable due to uncontrolled phase combinations of aluminium sulphate phases, leading to e.g. segregation or gel formation. Therefore, suspensions based on aluminium sulphate are generally not stable over a period of hours to months. Depending on the preparation and storage conditions, they may segregate, agglomerate or gel. Therefore, the stability problem needs to be solved by combining other components, and the performance of the accelerator is also considered.
Patent CN 111377638A discloses a liquid alkali-free accelerator for improving cohesiveness of sprayed concrete and a preparation method thereof. The modified attapulgite can stabilize the mixture and provide higher suspension force, the special charge-mechanical effect can play a role in suspending solids, particularly the suspension effect in a high-solid-content system is better, the viscosity of the system is not improved, and the use performance is not influenced, so that the high-solid-content liquid alkali-free accelerator can keep excellent suspension fluidity. Patent CN110922085A discloses a supersaturation suspension type alkali-free liquid accelerator for aluminum sulfate and a preparation method thereof. The problems of high aluminum sulfate content and poor stability of the prepared alkali-free liquid accelerator can be effectively solved through the synergistic effect of the organic acid complexing agent, the alcohol amine, the superfine sepiolite powder, the polyacrylamide, the pH regulator and the like. Patent CN 110963736A discloses a nano gel polymeric aluminum type liquid alkali-free accelerator and a preparation method thereof. The aluminum sulfate and the aluminum carbonate are used as main aluminum phase components, the formation of polyaluminum sulfate is realized by utilizing the double hydrolysis effect of the aluminum carbonate and obviously reducing the dosage of the aluminum sulfate, and thus the aluminum phase ion concentration of an alkali-free system is improved. The nanometer calcium silicate hydrate gel can promote the hydration of tricalcium silicate fast, raise the early strength of cement harmlessly, and raise the long term stability of the product together with organic amide stabilizer. Although the above patent technologies can achieve good stabilizing effects through the synergistic effect of the inorganic and/or organic components, the above patent technologies still have some disadvantages in the application effects of the product, such as improving the early strength of the concrete, reducing the rebound resilience of the shotcrete, and the convenience of applying the shotcrete.
The rebound rate of sprayed concrete is the ratio of the number of rebounded concrete to the total number of concrete, and is the proportion of the concrete which cannot be effectively attached to a sprayed surface. In the existing sprayed concrete construction, due to the reasons of unreasonable mix ratio, improper control of concrete working state, scientific control parameters of a sprayer and the like, the rebound rate is too large in the spraying process, so that a large amount of materials are wasted, the construction quality of the sprayed concrete is influenced, certain potential safety hazards are caused to a spraying hand, and the construction efficiency is reduced. Through the statistics of the relevant engineering of mass sprayed concrete, the rebound rate ranges from 20% to 30%, which is also a great waste for the total production of sprayed concrete. In order to improve the performance of sprayed concrete, reduce the rebound rate of the sprayed concrete and improve the molding quality of the sprayed concrete, the research work of the mix proportion of the sprayed concrete is also carried out continuously, and at present, the performance of the sprayed concrete is improved by adopting a method of adding mineral mixed materials, including mineral admixtures such as silica fume, fly ash and limestone micro powder. In the aspect of mix proportion design, a method of introducing a tackifying material is mostly adopted at home and abroad to increase the cohesiveness of the fresh concrete so as to reduce the rebound rate of the sprayed concrete. The solid mineral admixture or other organic materials are directly added into the concrete, although the cohesiveness of the concrete can be effectively improved, the addition of the solid mineral admixture or other organic materials before the spraying operation can cause that the premixed concrete pumped out by a pump can not be effectively sprayed out by a spraying machine, the requirement on the spraying machine is higher, and the pipe blockage of the spraying machine can be frequently caused.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a preparation method of a suspension type alkali-free liquid accelerator.
The invention also aims to provide a suspension type alkali-free liquid accelerator prepared by the method.
The suspension type alkali-free liquid accelerator disclosed by the invention adopts the amino-terminated hyperbranched polymer and the magnesium-aluminum layered double hydroxide as a suspension stabilizing system, can be used for suspending and stabilizing a high-concentration supersaturated aluminum sulfate solution system, can achieve a good accelerating effect and improve the early strength of concrete, and can reduce the rebound rate of sprayed concrete and effectively improve the pipe blockage phenomenon in the application process of the sprayed concrete. Has very good comprehensive use performance.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a suspension type alkali-free liquid accelerator comprises the following preparation steps:
(1) preparation of magnesium-aluminum layered double hydroxide:
dissolving magnesium salt and aluminum salt in a mixed solvent of water and N, N-dimethylformamide, adding an alkaline activator, stirring and mixing uniformly, carrying out hydrothermal reaction at the temperature of 80-160 ℃, and filtering, washing, drying and grinding a solid product to obtain magnesium-aluminum layered double hydroxide;
(2) preparation of amino-terminated hyperbranched polymer:
adding N, N-methylene-bisacrylamide and diethylenetriamine into an N, N-dimethylformamide solvent, then adding an alkaline catalyst, stirring and mixing uniformly, heating to 30-80 ℃, stirring for reaction, and evaporating low-boiling-point substances under reduced pressure after the reaction is finished to obtain an amino-terminated hyperbranched polymer;
(3) preparing a suspension type alkali-free liquid accelerator:
adding the magnesium-aluminum layered double hydroxide and the amino-terminated hyperbranched polymer into water, stirring and dispersing uniformly, then adding aluminum sulfate and a pH regulator, stirring and dispersing uniformly, and obtaining the suspension type alkali-free liquid accelerator.
Further, in the step (1), the magnesium salt is selected from magnesium nitrate, magnesium chloride or magnesium sulfate.
Further, the aluminum salt in step (1) is selected from aluminum nitrate, aluminum chloride or aluminum sulfate.
Further, the addition ratio of the magnesium salt and the aluminum salt in the step (1) is Mg2+/Al3+The molar ratio of (2-4): 1. Divalent metal Mg2+And trivalent metal Al3+Of (2)The proper proportion is favorable for generating a layered double hydroxide structure with large specific surface area.
Further, in the step (1), the alkaline activator is sodium hydroxide or potassium hydroxide.
Furthermore, the molar ratio of the N, N-methylene-bisacrylamide in the step (2) to the diethylenetriamine is 1 (1.2-2). The excessive addition of the diethylenetriamine is beneficial to the formation of a hyperbranched structure, and a large number of amino groups are distributed at the tail end of the hyperbranched structure, so that supersaturated aluminum sulfate can be dispersed better and stably, the hydration of C3A in cement is promoted, the generation of ettringite is accelerated, and the early strength of concrete is improved.
Further, in the step (2), the basic catalyst is sodium alkoxide (such as sodium ethoxide, sodium methoxide and the like), tertiary amine (such as triethanolamine and the like) or metal hydride (such as NaH and the like).
Further, in the step (3), the pH regulator is at least one selected from ethylenediamine tetraacetic acid, oxalic acid, citric acid, salicylic acid and phosphoric acid.
A suspension type alkali-free liquid accelerator is prepared by the method.
Further, the suspension type alkali-free liquid accelerator comprises the following components in percentage by mass:
the principle of the invention is as follows: the amino-terminated hyperbranched polymer is prepared by reacting N, N-methylene bisacrylamide and diethylenetriamine under the basic catalysis of a Michael addition reaction or diethylenetriamine and then serving as a stable system of supersaturated aluminum sulfate with magnesium-aluminum layered double hydroxide. The amino-terminated hyperbranched polymer has a typical molecular structure shown in the following formula I, and a large number of amide groups and amino groups contained in the amino-terminated hyperbranched polymer can effectively complex and stabilize an aluminum phase material, so that the stability of a suspension is remarkably improved. Meanwhile, a great amount of amino groups are distributed at the tail end of the branched structure of the amino-terminated hyperbranched polymer, so that the hydration of C3A in cement can be better promoted, and the ettringite is acceleratedThereby improving the early strength of the concrete. Layered Double Hydroxides (LDHs), also called hydrotalcite-like compounds, are mainly composed of magnesium octahedrons and aluminum octahedrons. The Mg-Al layered double hydroxide is formed by divalent Mg2+And trivalent Al3+The ionic constituent can be prepared by simple solvothermal or hydrothermal reaction. Due to the characteristics of special structure, high specific surface area, alkalescence and the like, the layered double hydroxide can further cooperate with the amino-terminated hyperbranched polymer to form an inorganic-organic polymer co-stabilization system and a tackifying system. The co-stabilizing system and the tackifying system of the inorganic-organic polymer can increase the cohesiveness of fresh concrete so as to reduce the rebound rate of sprayed concrete. And the magnesium-aluminum layered double hydroxide is used as an aluminum phase material to improve the early strength of the concrete to a certain extent. The hyperbranched polymer with the amino end has better rheological improvement property due to the hyperbranched structure, and can reduce the pipe blockage phenomenon of solid suspended materials to injection machinery.
Compared with the prior art, the invention has the beneficial effects that:
(1) the suspension type alkali-free liquid accelerator can stably suspend aluminum sulfate with the content of 50-60%, and has faster and better accelerating effect compared with the alkali-free liquid accelerator on the existing market.
(2) The invention adopts the magnalium layered double hydroxides with high dispersibility and high specific surface area to further cooperate with the amino-terminated hyperbranched polymer to form an inorganic-organic polymer co-stabilizing system and a tackifying system, and can increase the cohesiveness of fresh concrete so as to reduce the rebound rate of sprayed concrete.
(3) The magnesium-aluminum layered double hydroxide adopted by the invention is used as an aluminum phase material to improve the early strength of the concrete to a certain extent.
(4) The amino-terminated hyperbranched polymer adopted by the invention has better rheological improvement property due to the hyperbranched structure, and can reduce the pipe blockage phenomenon of solid suspended materials on injection machinery.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
The suspension type alkali-free liquid accelerator comprises the following components in percentage by mass:
the suspension type alkali-free liquid accelerator is prepared by the following method:
(1) preparation of magnesium-aluminum layered double hydroxide: mixing magnesium sulfate and aluminum sulfate as Mg2+/Al3+Dissolving the mixture in a molar ratio of 2:1 in a mixed solvent of water and N, N-dimethylformamide in a volume ratio of 1:2, adding sodium hydroxide, stirring and mixing uniformly, performing hydrothermal reaction at a temperature of 120-150 ℃, and filtering, washing, drying and grinding a solid product to obtain the nanoscale magnesium-aluminum layered double hydroxide.
(2) Preparation of amino-terminated hyperbranched polymer: adding N, N-methylene bisacrylamide and diethylenetriamine into an N, N-dimethylformamide solvent according to the molar ratio of 1:1.5, then adding sodium ethoxide with the mass of 0.2% of that of the N, N-methylene bisacrylamide, stirring and mixing uniformly, heating to 45 ℃, stirring and reacting for 6 hours, and after the reaction is finished, evaporating low-boiling-point substances under reduced pressure to obtain a viscous liquid amino-terminated hyperbranched polymer (the detected weight-average molecular weight is about 9600).
(3) Preparing a suspension type alkali-free liquid accelerator: adding the obtained magnesium-aluminum layered double hydroxide and the amino-terminated hyperbranched polymer into water, stirring and dispersing uniformly, then adding aluminum sulfate and citric acid serving as a pH regulator, and stirring and dispersing uniformly to obtain the suspension type alkali-free liquid accelerator.
Example 2
The suspension type alkali-free liquid accelerator comprises the following components in percentage by mass:
the suspension type alkali-free liquid accelerator is prepared by the following method:
(1) preparation of magnesium-aluminum layered double hydroxide: mixing magnesium sulfate and aluminum sulfate as Mg2+/Al3+Dissolving the mixture in a mixed solvent of water and N, N-dimethylformamide in a volume ratio of 1:2 at a molar ratio of 3:1, adding sodium hydroxide, stirring and mixing uniformly, performing hydrothermal reaction at a temperature of 120-150 ℃, and filtering, washing, drying and grinding a solid product to obtain the nanoscale magnesium-aluminum layered double hydroxide.
(2) Preparation of amino-terminated hyperbranched polymer: adding N, N-methylene bisacrylamide and diethylenetriamine into an N, N-dimethylformamide solvent according to the molar ratio of 1:1.5, then adding triethanolamine with the mass of 0.5% of that of the N, N-methylene bisacrylamide, uniformly stirring and mixing, heating to 60 ℃, stirring and reacting for 12 hours, and after the reaction is finished, evaporating low-boiling-point substances under reduced pressure to obtain a viscous liquid amino-terminated hyperbranched polymer (the detected weight-average molecular weight is about 11400).
(3) Preparing a suspension type alkali-free liquid accelerator: adding the obtained magnesium-aluminum layered double hydroxide and the amino-terminated hyperbranched polymer into water, stirring and dispersing uniformly, then adding aluminum sulfate and a pH regulator, namely ethylene diamine tetraacetic acid, and stirring and dispersing uniformly to obtain the suspension type alkali-free liquid accelerator.
Example 3
The suspension type alkali-free liquid accelerator comprises the following components in percentage by mass:
the suspension type alkali-free liquid accelerator is prepared by the following method:
(1) layered double-layer magnesium-aluminum alloyPreparation of the metal hydroxide: mixing magnesium sulfate and aluminum sulfate as Mg2+/Al3+Dissolving the mixture in a mixed solvent of water and N, N-dimethylformamide in a volume ratio of 1:2 at a molar ratio of 4:1, adding sodium hydroxide, stirring and mixing uniformly, performing hydrothermal reaction at a temperature of 120-150 ℃, and filtering, washing, drying and grinding a solid product to obtain the nanoscale magnesium-aluminum layered double hydroxide.
(2) Preparation of amino-terminated hyperbranched polymer: adding N, N-methylene bisacrylamide and diethylenetriamine into an N, N-dimethylformamide solvent according to the molar ratio of 1:1.2, then adding sodium methoxide with the mass of 0.5% of that of the N, N-methylene bisacrylamide, uniformly stirring and mixing, heating to 50 ℃, stirring and reacting for 4 hours, and evaporating low-boiling-point substances under reduced pressure after the reaction is finished to obtain the elastomer-shaped amino-terminated hyperbranched polymer (the detected weight average molecular weight is about 17800).
(3) Preparing a suspension type alkali-free liquid accelerator: adding the obtained magnesium-aluminum layered double hydroxide and the amino-terminated hyperbranched polymer into water, stirring and dispersing uniformly, then adding aluminum sulfate and a pH regulator phosphoric acid, stirring and dispersing uniformly, and obtaining the suspension type alkali-free liquid accelerator.
Comparative example 1
Compared with the embodiment 2, the mixed system of the amino-terminated hyperbranched polymer and the magnalium layered double hydroxide is replaced by the organic amine compound triisopropanolamine and the thickening agent polyacrylamide as the stability promoting system, and the specific components and the preparation method are as follows:
the suspension type alkali-free liquid accelerator of the comparative example was prepared by the following method:
adding aluminum sulfate into water, heating, stirring and dissolving uniformly, then adding triisopropanolamine, polyacrylamide and ethylene diamine tetraacetic acid, stirring and mixing uniformly, and cooling to room temperature to obtain the suspension type alkali-free liquid accelerator of the comparative example.
Comparative example 2
A commercially available alkali-free liquid accelerator was used, and the solid content was 46.5%.
The alkali-free liquid accelerator obtained in the above examples and comparative examples was subjected to a performance test:
1. testing of setting time of cement paste, cement mortar strength and rebound rate of sprayed concrete
The setting accelerators of examples 1 to 3 and comparative examples 1 to 2 were added to the cement paste in an amount of 6% by weight based on the weight of the cement, and commercially available ordinary portland cement was selected. And (3) carrying out cement paste setting time and cement mortar strength tests according to the requirements of the standard GB/T35159 and 2017 accelerator for sprayed concrete. The rebound resilience test of shotcrete was performed as specified in the industry standard JGJ/T372-2016 technical Specification for shotcrete application.
2. Stability test
And standing at normal temperature for precipitation.
The test results are shown in Table 1.
TABLE 1
The results in table 1 clearly show that magnesium-aluminum layered double hydroxides cooperate with amino-terminated hyperbranched polymers to form an inorganic-organic polymer co-stabilization system and a tackifying system, and compared with a stabilization system of alcohol amine and polyacrylamide and a common commercially available alkali-free liquid accelerator system, the high-concentration supersaturated aluminum sulfate suspension has the advantages of remarkably improving the storage stability, obviously shortening the setting time, further improving the early strength of concrete and reducing the rebound rate. And no pipe blockage phenomenon is found in the using process, and slight pipe blockage and nozzle material residue occur when the high-concentration aluminum sulfate suspension type alkali-free liquid accelerator in the comparative example 1 is adopted, so that the mixing and stabilizing system can effectively improve the rheological property and the spraying performance of the material.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A preparation method of a suspension type alkali-free liquid accelerator is characterized by comprising the following preparation steps:
(1) preparation of magnesium-aluminum layered double hydroxide:
dissolving magnesium salt and aluminum salt in a mixed solvent of water and N, N-dimethylformamide, adding an alkaline activator, stirring and mixing uniformly, carrying out hydrothermal reaction at the temperature of 80-160 ℃, and filtering, washing, drying and grinding a solid product to obtain magnesium-aluminum layered double hydroxide;
(2) preparation of amino-terminated hyperbranched polymer:
adding N, N-methylene-bisacrylamide and diethylenetriamine into an N, N-dimethylformamide solvent, then adding an alkaline catalyst, stirring and mixing uniformly, heating to 30-80 ℃, stirring for reaction, and evaporating low-boiling-point substances under reduced pressure after the reaction is finished to obtain an amino-terminated hyperbranched polymer;
(3) preparing a suspension type alkali-free liquid accelerator:
adding the magnesium-aluminum layered double hydroxide and the amino-terminated hyperbranched polymer into water, stirring and dispersing uniformly, then adding aluminum sulfate and a pH regulator, stirring and dispersing uniformly to obtain the suspension type alkali-free liquid accelerator;
the mass percentage of each component in the step (3) is as follows:
50 to 60 percent of aluminum sulfate;
5 to 10 percent of magnesium-aluminum layered double hydroxide;
0.5 to 5 percent of amino-terminated hyperbranched polymer;
0.2 to 2 percent of pH regulator;
the balance of water.
2. The method for preparing the suspension type alkali-free liquid accelerator as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the magnesium salt is selected from magnesium nitrate, magnesium chloride or magnesium sulfate.
3. The method for preparing the suspension type alkali-free liquid accelerator as claimed in claim 1, wherein the method comprises the following steps: the aluminum salt in the step (1) is selected from aluminum nitrate, aluminum chloride or aluminum sulfate.
4. The method for preparing the suspension type alkali-free liquid accelerator as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the addition ratio of the magnesium salt to the aluminum salt is Mg2+/Al3+The molar ratio of (2-4): 1.
5. The method for preparing the suspension type alkali-free liquid accelerator as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the alkaline activator is sodium hydroxide or potassium hydroxide.
6. The method for preparing the suspension type alkali-free liquid accelerator as claimed in claim 1, wherein the method comprises the following steps: the molar ratio of the N, N-methylene bisacrylamide to the diethylenetriamine in the step (2) is 1 (1.2-2).
7. The method for preparing the suspension type alkali-free liquid accelerator as claimed in claim 1, wherein the method comprises the following steps: in the step (2), the alkaline catalyst is sodium alkoxide, tertiary amine or metal hydride.
8. The method for preparing the suspension type alkali-free liquid accelerator as claimed in claim 1, wherein the method comprises the following steps: in the step (3), the pH regulator is at least one selected from ethylenediamine tetraacetic acid, oxalic acid, citric acid, salicylic acid and phosphoric acid.
9. A suspension type alkali-free liquid accelerator is characterized in that: prepared by the method of any one of claims 1 to 8.
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| CN115703671A (en) * | 2021-08-11 | 2023-02-17 | 贵州省安顺开发区三合砼业有限公司 | Inorganic salt alkali return prevention accelerator and preparation method thereof |
| CN114436559B (en) * | 2022-03-11 | 2022-09-23 | 北京工业大学 | Method for preparing liquid alkali-free accelerator by ring opening of cyclic amide monomer |
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