CN110963732A - Environment-friendly alkali-free liquid accelerator and normal-temperature preparation method thereof - Google Patents
Environment-friendly alkali-free liquid accelerator and normal-temperature preparation method thereof Download PDFInfo
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- CN110963732A CN110963732A CN201911366257.8A CN201911366257A CN110963732A CN 110963732 A CN110963732 A CN 110963732A CN 201911366257 A CN201911366257 A CN 201911366257A CN 110963732 A CN110963732 A CN 110963732A
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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
Abstract
The invention discloses an environment-friendly alkali-free liquid accelerator and a normal-temperature preparation method thereof; the accelerator comprises the following components in percentage by mass: 45-60% of aluminum sulfate, 5-10% of alcohol amine, 0-2.5% of complexing agent, 0.5-2% of organic acid and the balance of water; the method for preparing the accelerator at normal temperature comprises the following steps: weighing the components according to the mass ratio; mixing alcohol amine, complexing agent and water and stirring for a certain time to form solution A; adding aluminum sulfate into the solution A, and continuously stirring for a certain time to form solution B; adding organic acid into the solution B, and continuously stirring for a certain time to obtain the alkali-free liquid accelerator. The invention can prepare the liquid accelerator at normal temperature, uses few raw materials during preparation, does not need to adopt dripping equipment, and has no harmful fluoride ions and chloride ions after preparation.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to an environment-friendly alkali-free liquid accelerator for sprayed concrete and a normal-temperature preparation method thereof.
Background
The accelerator is an additive capable of quickly setting and hardening concrete, is an important material in sprayed concrete construction, and has the main functions of accelerating the setting and hardening speed of the sprayed concrete, reducing rebound loss, preventing the sprayed concrete from falling off due to gravity, increasing the once spraying thickness and shortening the interval time between sprayed layers. The accelerator is mainly used for projects such as spray anchor support, railways, tunnels, water conservancy, traffic, mining and the like. The research of the accelerator is that the powdery accelerator has the defects of large rebound quantity, large dust, uneven doping, poor operation environment and great harm influence on the health of constructors and the environment. The alkaline liquid accelerator has high solid content, good stability, good adaptability to different types of cement and high early strength; but the influence of the concrete on the later strength is large, and the strength loss in 28 days can reach more than 30%. The negative influence of alkali-aggregate reaction caused by high alkali content still seriously restricts the engineering application of the accelerating agent. Along with the requirement of the current construction unit on the greening of the sprayed concrete construction, the domestic technology is promoted to carry out a great deal of research on an alkali-free liquid accelerator system taking aluminum sulfate as a main accelerating component. However, in view of the limitation of raw material systems, most of the alkali-free accelerators are prepared by adding various organic and inorganic materials to modify the solubility of aluminum sulfate or the performance of the accelerator, wherein the most widely used complexing agents such as organic amine, alcohol amine, organic carboxylic acid and polyalcohol and inorganic raw materials such as fluoride, organic acid and magnesium sulfate are used, and then adding a proper amount of stabilizer and a certain amount of viscosity modifier to improve the stability of the alkali-free liquid accelerator, and combining a certain synthesis process under a certain temperature condition. The main problems of the method are as follows: the existing alkali-free liquid accelerator has the defects that the variety of raw materials required in the preparation process is great, the material cost is increased, and liquid dripping equipment needs to be additionally purchased, so that the equipment purchasing cost is increased, and the process cost of the accelerator is increased; meanwhile, in the existing alkali-free setting accelerator, in order to improve the stability of the accelerator, fluoride such as hydrofluoric acid, magnesium fluoride, sodium fluoride and the like is added, so that the produced accelerator contains a large amount of harmful fluorine ions and alkaline substances, and certain harm is caused to the environment, production and constructors. In the existing accelerator preparation process, heating treatment is usually carried out for promoting dissolution or reaction, and the heating process in the production process can increase the production energy consumption and is not beneficial to reducing the production cost.
Disclosure of Invention
The invention aims to provide an environment-friendly alkali-free liquid accelerator which is prepared from a few kinds of raw materials, is produced at normal temperature and is free of harmful fluoride ions and chloride ions after preparation, and also aims to provide a normal-temperature preparation method of the environment-friendly alkali-free liquid accelerator which can be prepared at normal temperature and can effectively reduce the production cost.
The technical scheme of the invention is as follows:
an environment-friendly alkali-free liquid accelerator comprises the following components in percentage by mass:
45-60% of aluminum sulfate, 5-10% of alcohol amine, 0-2.5% of complexing agent, 0.5-2% of organic acid and the balance of water.
Further, the alcohol amine is diethanolamine or a mixture of diethanolamine and triethanolamine.
Further, the mass ratio of the diethanolamine to the triethanolamine is 1: 0.5-1.
Further, the complexing agent is aluminum citrate.
Further, the organic acid is oxalic acid.
A preparation method of an environment-friendly alkali-free liquid accelerator comprises the following steps:
(1) weighing 45-60% of aluminum sulfate, 5-10% of alcohol amine, 0-2.5% of complexing agent, 0.5-2% of organic acid and the balance of water according to the mass ratio;
(2) mixing alcohol amine, a complexing agent and water, and stirring for 0.5-1 h to form solution A;
(3) adding aluminum sulfate into the solution A, and continuously stirring for 2.5-6 hours to form solution B;
(4) adding organic acid into the solution B, and continuously stirring for 1h to obtain the alkali-free liquid accelerator.
Further, the stirring speed in the steps (2), (3) and (4) is controlled to be 1800-2500 r/min.
The invention has the beneficial effects that:
the accelerator only consists of aluminum sulfate, alcohol amine, complexing agent, organic acid and water on the raw materials, so that the needed raw materials are few, and the raw material cost can be reduced; fluoride is not contained in the raw materials, harmful fluoride ions and chloride ions are not contained in the prepared accelerator, and the prepared accelerator is more environment-friendly and safer; based on the selection of raw materials and proportion, dripping equipment is not needed in the preparation process, so that equipment purchase cost can be reduced; the accelerator can be prepared at normal temperature, the normal-temperature preparation is realized by improving the adding sequence of raw materials and selecting process parameters in the process, the preparation method is simple and convenient, dripping equipment is not needed, heating treatment is not needed, the energy consumption of process production can be effectively reduced, the production cost is effectively reduced, and meanwhile, the prepared accelerator completely meets the requirements of GB/T35159-2017 accelerator for sprayed concrete.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention is further described in detail with reference to the following examples.
An environment-friendly alkali-free liquid accelerator comprises the following components in percentage by mass:
45-60% of aluminum sulfate, 5-10% of alcohol amine, 0-2.5% of complexing agent, 0.5-2% of organic acid and the balance of water; wherein, aluminum sulfate is the main coagulation accelerating component; the alcohol amine is used for improving the early strength of concrete, the alcohol amine can be selected from diethanol amine or a mixture of diethanol amine and triethanol amine, and meanwhile, the alcohol amine can be complexed with aluminum ions in a solution to form a water-soluble product, so that the dissolving amount of aluminum sulfate can be improved, and the alcohol amine plays a role of a stabilizer, if the mixture of diethanol amine and triethanol amine is selected, the mass ratio of the diethanol amine to the triethanol amine is controlled to be 1: 0.5-1, and an accelerator meeting performance requirements cannot be obtained when the triethanol amine is used alone in the formula; the complexing agent is aluminum citrate, so that the stability of the accelerating agent can be improved; the organic acid is oxalic acid which can be used as a coagulation promoting component and a pH regulator; the aluminum citrate can play a certain role in promoting the dissolution of aluminum sulfate in the process of preparing the accelerator, and can reduce the stirring time of the solution after the aluminum sulfate is added. The diethanol amine has certain complexation, so that aluminum citrate can be not added according to production requirements in the actual preparation process of the accelerator based on the complexation of the diethanol amine and a mode of increasing stirring time.
A normal-temperature preparation method of an environment-friendly alkali-free liquid accelerator comprises the following steps:
(1) weighing 45-60% of aluminum sulfate, 5-10% of alcohol amine, 0-2.5% of complexing agent, 0.5-2% of organic acid and the balance of water according to the mass ratio; wherein, the alcohol amine can be diethanol amine or a mixture of diethanol amine and triethanol amine, and the mass ratio of the diethanol amine to the triethanol amine is 1: 0.5-1 when the diethanol amine and the triethanol amine are mixed for use; the complexing agent is aluminum citrate; the organic acid is oxalic acid.
(2) Mixing the weighed alcohol amine, complexing agent and water, stirring for 0.5-1 h, controlling the stirring speed to be 1800-2500 r/min during stirring, and stirring to form solution A; in the conventional operation process, a heating mode is usually adopted for promoting the dissolution of aluminum sulfate in water, so that the solubility of the aluminum sulfate in the water is improved; the method mixes the alcohol amine, the complexing agent and the water at normal temperature, and can promote the dissolution of the aluminum sulfate by utilizing the complexing action and improve the stability of the accelerator when the aluminum sulfate is added subsequently.
(3) Adding aluminum sulfate into the solution A, continuously stirring for 2.5-6 h, controlling the stirring speed to be 1800-2500 r/min during stirring, and stirring to form solution B; because the aluminum citrate has certain complexation, the stirring time in the step can be shortened after a proper amount of aluminum citrate is added, if the aluminum citrate is not added, the stirring time can be properly increased to improve the stability of the accelerator, the use of raw materials can be further reduced without adding the aluminum citrate, and the reduction of the production cost is facilitated.
(4) Adding oxalic acid into the solution B, continuously stirring for 1h, controlling the stirring speed to be 1800-2500 r/min during stirring, and obtaining the alkali-free liquid accelerator after stirring.
The four steps are all prepared at normal temperature, heating operation is not needed in the whole process, dripping equipment is not needed, and the process cost for preparing the accelerator can be effectively reduced.
Example 1:
(1) weighing 52% of aluminum sulfate, 6% of diethanolamine, 2% of aluminum citrate, 1% of oxalic acid and the balance of water according to the mass ratio;
(2) mixing diethanolamine, aluminum citrate and water, stirring for 0.5h, controlling the stirring speed at 2000r/min during stirring, and stirring to form solution A;
(3) adding aluminum sulfate into the solution A, continuously stirring, controlling the stirring speed to be 2000r/min and the stirring time to be 3h during stirring, and stirring to form solution B;
(4) adding oxalic acid into the solution B, continuously stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and obtaining the alkali-free liquid accelerator after stirring.
Example 2:
(1) weighing 55% of aluminum sulfate, 6% of diethanolamine, 2% of aluminum citrate, 1% of oxalic acid and the balance of water according to the mass ratio;
(2) mixing diethanolamine, aluminum citrate and water, stirring for 0.5h, controlling the stirring speed at 2000r/min during stirring, and stirring to form solution A;
(3) adding aluminum sulfate into the solution A, continuously stirring, controlling the stirring speed to be 2000r/min and the stirring time to be 3h during stirring, and stirring to form solution B;
(4) adding oxalic acid into the solution B, continuously stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and obtaining the alkali-free liquid accelerator after stirring.
Example 3:
(1) weighing 55% of aluminum sulfate, 3% of diethanolamine, 3% of triethanolamine, 2% of aluminum citrate, 1% of oxalic acid and the balance of water according to the mass ratio;
(2) mixing diethanolamine, aluminum citrate and water, stirring for 0.5h, controlling the stirring speed at 2000r/min during stirring, and stirring to form solution A;
(3) adding aluminum sulfate into the solution A, continuously stirring, controlling the stirring speed to be 2000r/min and the stirring time to be 3h during stirring, and stirring to form solution B;
(4) adding oxalic acid into the solution B, continuously stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and obtaining the alkali-free liquid accelerator after stirring.
Example 4:
(1) weighing 55% of aluminum sulfate, 4% of diethanolamine, 2% of triethanolamine, 2% of aluminum citrate, 1% of oxalic acid and the balance of water according to the mass ratio;
(2) mixing diethanolamine, aluminum citrate and water, stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and stirring to form solution A;
(3) adding aluminum sulfate into the solution A, continuously stirring, controlling the stirring speed to be 2000r/min and the stirring time to be 3h during stirring, and stirring to form solution B;
(4) adding oxalic acid into the solution B, continuously stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and obtaining the alkali-free liquid accelerator after stirring.
Example 5:
(1) weighing 55% of aluminum sulfate, 4% of diethanolamine, 4% of triethanolamine, 2% of aluminum citrate, 1% of oxalic acid and the balance of water according to the mass ratio;
(2) mixing diethanolamine and aluminum citrate with water, stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and stirring to form solution A;
(3) adding aluminum sulfate into the solution A, continuously stirring, controlling the stirring speed to be 2000r/min and the stirring time to be 3h during stirring, and stirring to form solution B;
(4) adding oxalic acid into the solution B, continuously stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and obtaining the alkali-free liquid accelerator after stirring.
Example 6:
(1) weighing 55% of aluminum sulfate, 6% of diethanolamine, 1% of oxalic acid and the balance of water according to the mass ratio;
(2) mixing diethanolamine and water, stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and stirring to form solution A;
(3) adding aluminum sulfate into the solution A, continuously stirring, controlling the stirring speed to be 2000r/min and the stirring time to be 5h during stirring, and stirring to form solution B;
(4) adding oxalic acid into the solution B, continuously stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and obtaining the alkali-free liquid accelerator after stirring.
Example 7:
(1) weighing 55% of aluminum sulfate, 6% of triethanolamine and 1% of oxalic acid according to the mass ratio, and supplementing the balance by water;
(2) mixing diethanolamine and water, stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and stirring to form solution A;
(3) adding aluminum sulfate into the solution A, continuously stirring, controlling the stirring speed to be 2000r/min and the stirring time to be 5h during stirring, and stirring to form solution B;
(4) adding oxalic acid into the solution B, continuously stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and obtaining the alkali-free liquid accelerator after stirring.
Example 8:
(1) weighing 57% of aluminum sulfate, 7% of diethanolamine, 1% of oxalic acid and the balance of water according to the mass ratio;
(2) mixing diethanolamine and water, stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and stirring to form solution A;
(3) adding aluminum sulfate into the solution A, continuously stirring, controlling the stirring speed to be 2000r/min and the stirring time to be 5h during stirring, and stirring to form solution B;
(4) adding oxalic acid into the solution B, continuously stirring for 1h, controlling the stirring speed at 2000r/min during stirring, and obtaining the alkali-free liquid accelerator after stirring.
The mixing amount of the accelerator prepared by the method is 6-9% of the cement amount; the performance test is carried out by applying the above examples 1 to 8 in the reference cement according to the doping amount of 6 percent; the test results are shown in table 1;
table 1: examples 1-8 Performance test results for use in Cement
As can be seen from Table 1, examples 1, 2, 3, 4, 5, 6 and 8 all satisfied the requirements of GB/T35159-2017 accelerator for shotcrete and had good stability; the 1d compressive strength of the example 7 is less than 7, and does not meet the requirement of GB/T35159-2017, so that the accelerator meeting the requirement cannot be obtained by singly using triethanolamine in the components disclosed by the invention; in the embodiments 3, 4 and 5, a mixed mode of diethanolamine and triethanolamine is adopted, and meanwhile, the diethanolamine and triethanolamine are controlled in a mass ratio of 1: 0.5-1, so that the prepared accelerator can meet the requirement of GB/T35159-2017, and the triethanolamine which is used alone cannot meet the requirement but can still meet the requirement of GB/T35159-2017 by being mixed with the diethanolamine and controlled in a certain proportion range; as can be seen from the comparison between the examples 1 to 5 and the examples 6 and 8, the stirring time after adding aluminum sulfate can be reduced after using aluminum citrate, and the accelerator meeting the GB/T35159-2017 requirements can be obtained by increasing the stirring time without adding aluminum citrate, and the accelerator can be rapidly prepared at normal temperature in the actual production process, the aluminum citrate can be added during the preparation, so that the preparation cost of the accelerator can be effectively saved if needed, and the aluminum citrate can be optionally not added; comparing examples 6 and 8, it can be seen that the amount of diethanolamine used in example 6 is less on the premise of meeting the performance requirements, which can further reduce the production cost; since the enterprise needs to balance the cost and efficiency problems, the invention takes the low-cost accelerator prepared in example 6 as an example, and tests the performance results and the adaptability to cement at different mixing amounts, and the results are shown in table 2:
table 2: example 6 Performance results and Adaptation results to Cement at different loadings
As can be seen from Table 2, the accelerator prepared in example 6 meets the standard requirements under different parameters and has good adaptability to different cements.
Claims (7)
1. The environment-friendly alkali-free liquid accelerator is characterized by comprising the following components in percentage by mass:
45-60% of aluminum sulfate, 5-10% of alcohol amine, 0-2.5% of complexing agent, 0.5-2% of organic acid and the balance of water.
2. The environment-friendly alkali-free liquid accelerator as claimed in claim 1, wherein the alcohol amine is diethanolamine or a mixture of diethanolamine and triethanolamine.
3. The environment-friendly alkali-free liquid accelerator as claimed in claim 2, wherein the mass ratio of the diethanolamine to the triethanolamine is 1: 0.5-1.
4. The environment-friendly alkali-free liquid accelerator as claimed in claim 1, wherein the complexing agent is aluminum citrate.
5. The environment-friendly alkali-free liquid accelerator as claimed in claim 1, wherein the organic acid is oxalic acid.
6. The preparation method of the environment-friendly alkali-free liquid accelerator as claimed in claim 1, which comprises the following steps:
(1) weighing 45-60% of aluminum sulfate, 5-10% of alcohol amine, 0-2.5% of complexing agent, 0.5-2% of organic acid and the balance of water according to the mass ratio;
(2) mixing alcohol amine, a complexing agent and water, and stirring for 0.5-1 h to form solution A;
(3) adding aluminum sulfate into the solution A, and continuously stirring for 2.5-6 hours to form solution B;
(4) adding organic acid into the solution B, and continuously stirring for 1h to obtain the alkali-free liquid accelerator.
7. The method for preparing the environment-friendly alkali-free liquid accelerator at normal temperature as claimed in claim 6, wherein the stirring rotation speed during stirring in the steps (2), (3) and (4) is controlled to be 1800-2500 r/min.
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|---|---|---|---|---|
| CN111606595A (en) * | 2020-06-10 | 2020-09-01 | 竹鹏翔 | Preparation method of alkali-free liquid accelerator |
| CN112479620A (en) * | 2020-12-03 | 2021-03-12 | 五家渠格辉新材料有限责任公司 | Fluoride-free alkali-free accelerator and preparation method thereof |
| CN113213805A (en) * | 2021-03-31 | 2021-08-06 | 山西佳维新材料股份有限公司 | Quick early-strength alkali-free fluorine-free chlorine-free liquid accelerator and preparation method thereof |
| CN113264704A (en) * | 2021-07-08 | 2021-08-17 | 山西佳维新材料股份有限公司 | Alkali-free fluorine-free chlorine-free liquid accelerator and preparation method and application thereof |
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