Preparation method of C-S-H seed crystal type super early strength agent as well as product and application of C-S-H seed crystal type super early strength agent

Abstract

The invention relates to a preparation method of a C-S-H seed crystal type super early strength agent as well as a product and application of the C-S-H seed crystal type super early strength agent, and belongs to the technical field of production of cement-based materials. According to the preparation method, the C-S-H seed crystal type super early strength agent is obtained by mainly utilizing a microwave irradiation principle and taking a siliceous raw material, a calcium raw material, a dispersing agent, an organic complexing exciting agent and water as raw materials to react. The preparation method provided by the invention is short in reaction time, and the synthesized C-S-H seed crystal type super early strength agent has the characteristics of good early strength effect, good stability, greenness and harmlessness, can be widely applied to various product concrete and cast-in-place concrete projects, and has wide research background and important significance in the field of synthesis of composite materials such as concrete admixtures.

Description

Technical Field

[0001] The invention belongs to the technical field of building materials and relates to a preparation method of a CSH seed crystal type super early strength agent and a product and application thereof. Background Art

[0002] Microwave synthesis technology is an efficient, energy-saving and environmentally friendly material preparation method, which has been widely used in many fields in recent years. As a widely used building material, the improvement of concrete performance has an important impact on the quality and durability of construction projects. The rapid setting of concrete is its key performance indicator, which is directly related to the construction speed of the project. Therefore, the development of an additive that can shorten the setting time of concrete has important practical significance.

[0003] Traditional concrete super early strength agents are mostly prepared by chemical synthesis methods, which usually require long reaction times and high energy consumption, and may produce byproducts that are harmful to the environment during the production process. Therefore, developing a more efficient and environmentally friendly preparation method is crucial for the sustainable development of concrete additives.

[0004] As a new synthesis technology, microwave synthesis has the advantages of short reaction time, low energy consumption and mild reaction conditions. In the field of material synthesis, microwave synthesis has been proven to increase the reaction rate and improve the purity and performance of the product. Therefore, applying microwave synthesis technology to the preparation of concrete super early strength agent is expected to develop a new type of efficient and environmentally friendly concrete additive. Summary of the invention

[0005] In view of this, one of the objects of the present invention is to provide a method for preparing a CSH seed crystal type super early strength agent; a second object of the present invention is to provide a CSH seed crystal type super early strength agent; a third object of the present invention is to provide an application of a CSH seed crystal type super early strength agent in finished concrete, cast-in-place concrete, and mortar.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] 1. A method for preparing a CSH seed crystal type super early strength agent, the preparation method comprising the following steps:

[0008] (1) adding an aqueous solution of a dispersant having a mass fraction of 10.0% to 30% to a siliceous raw material solution in a three-necked flask in a microwave solid-liquid phase synthesizer, stirring to make the mixture uniform, and then subjecting the mixture to microwave reaction to obtain a reaction intermediate solution I;

[0009] (2) adding the calcium raw material solution into a three-necked flask to react, and keeping the temperature for 30 to 90 minutes after the reaction is completed to obtain a reaction intermediate solution II;

[0010] (3) adding an aqueous solution of an organic complexing activator with a mass fraction of 1% to 2% to the reaction intermediate solution II, stirring the mixture to react and uniformly mixing, and then transferring the mixture to a microwave solid-liquid phase synthesizer to continue the microwave reaction. After cooling, the mixture is taken out to obtain a CSH seed crystal type super early strength agent.

[0011] Preferably, in step (1), the mass ratio of the siliceous raw material to water in the siliceous raw material solution is 1:5-20;

[0012] In step (2), the mass ratio of the calcium raw material to water in the calcium raw material solution is 1:5-20.

[0013] Preferably, in step (2), the calcium raw material solution is added through a funnel or a syringe pump.

[0014] Preferably, in step (1), the stirring speed is 1000 r / min to 1500 r / min, and the microwave reaction conditions are: after heating to 40° C. to 85° C. within 5 to 10 minutes, microwave reaction is carried out at a power of 400 W to 800 W and a speed of 1000 r / min to 1500 r / min for 30 to 90 seconds;

[0015] In step (2), the stirring speed is 1000 r / min to 1500 r / min, the dropping speed is 0.1 ml / s to 0.5 ml / s, and the reaction time is 10 to 60 min;

[0016] In step (3), the microwave reaction conditions are: after heating to 80°C to 95°C, react at a power of 600W to 800W and a rotation speed of 1000r / min to 1500 / min for 30 to 60s.

[0017] 2. The CSH seed crystal type super early strength agent prepared according to the above preparation method, wherein the super early strength agent comprises a siliceous raw material, a calcium raw material, a dispersant, and an organic complexing activator;

[0018] The molar ratio of the silicon raw material, the calcium raw material, the dispersant and the organic complex activator is 0.8-1.7:1:0.1-0.5:0.01-0.05.

[0019] Preferably, the siliceous raw material includes any one or more of sodium silicate, silicon acetate, ethyl orthosilicate or silica ash.

[0020] Preferably, the calcium raw material includes any one or more of calcium nitrate, calcium chloride, calcium sulfate or calcium hydroxide.

[0021] Preferably, the dispersant includes any one or more of polycarboxylate ethers, polycarboxylates or polycarboxylic acid-polyether copolymers.

[0022] Preferably, the organic complexing activator includes any one or more of acrylamide, acrylic acid, maleic anhydride, vinyl pyridine, vinyl sulfonic acid or sodium styrene sulfonate.

[0023] 3. Application of the above CSH seed type super early strength agent in finished concrete, cast-in-place concrete and mortar.

[0024] The beneficial effects of the present invention are:

[0025] 1. The present invention discloses a CSH seed crystal type super early strength agent, which comprises a siliceous raw material, a calcium raw material, a dispersant and an organic complex activator, and has the advantages of effectively shortening the setting time of concrete and high early strength of concrete.

[0026] 2. The present invention also discloses a method for preparing a CSH seed crystal type super early strength agent, which is mainly prepared by microwave synthesis. The production process is environmentally friendly and efficient, and meets the requirements of green and sustainable development. The preparation method of the present invention can achieve rapid reaction of raw materials in a short time through microwave heating, and prepare a concrete additive with excellent performance, thereby improving the construction efficiency and quality of construction projects, and has good application prospects in finished concrete, cast-in-place concrete, and mortar. In addition, the preparation method of the present invention also has the characteristics of simple synthesis, short time and high efficiency.

[0027] Other advantages, objectives and features of the present invention will be described in the following description to some extent, and to some extent, will be obvious to those skilled in the art based on the following examination and study, or can be taught from the practice of the present invention. The objectives and other advantages of the present invention can be realized and obtained through the following description. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to make the purpose, technical solutions and advantages of the present invention more clear, the present invention will be described in detail below in conjunction with the accompanying drawings, wherein:

[0029] Figure 1 This is a diagram of the preparation device of CSH seed crystal type super early strength agent, wherein 1 is a funnel, 2 is a microwave instrument, 3 is a three-necked flask, 4 is a reactant, and 5 is a magnetic stirrer. DETAILED DESCRIPTION

[0030] The following describes the embodiments of the present invention by specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention. It should be noted that the illustrations provided in the following embodiments only illustrate the basic concept of the present invention in a schematic manner, and the following embodiments and features in the embodiments can be combined with each other without conflict.

[0031] The preparation device of CSH seed crystal type super early strength agent in the following embodiments is as follows Figure 1 As shown, 1 is a funnel, 2 is a microwave, 3 is a three-necked flask, 4 is a reactant, and 5 is a magnetic stirrer.

[0032] Example 1

[0033] A CSH seed crystal type super early strength agent, the specific preparation method is as follows:

[0034] (1) 111.66 g of sodium silicate was dissolved in 600 g of tap water, and the mixture was stirred for 50 s to obtain a sodium silicate solution. 9.988 g of polycarboxylate ether was added as a dispersant, and the mixture was stirred to obtain a uniform mixture. The mixture was heated to 85° C. within 7 min, and magnetic stirring was performed at a speed of 1500 r / min. A microwave reaction was performed at a microwave power of 600 W for 50 s to obtain a reaction intermediate solution I.

[0035] (2) 33.2952 g of calcium nitrate was dissolved in 300 g of tap water, stirred for 50 s to mix evenly to obtain a calcium nitrate solution, and the solution was added dropwise to the three-necked flask containing the reaction intermediate solution I at a rate of 0.1 ml / s through a syringe pump. The reaction time was 30 min, and then the solution was kept warm and cooled for 30 min to obtain a reaction intermediate solution II;

[0036] (3) Add 1% acrylamide by mass to the reaction intermediate solution II, stir for 45 seconds to make it evenly mixed, stir for 45 seconds to make it evenly mixed, and then place it in a microwave solid-liquid phase synthesizer, heat it to 85° C. and stir it at a speed of 1000 r / min, react for 10 minutes at a microwave power of 600 W, and take it out after cooling to obtain a CSH seed crystal type super early strength agent.

[0037] Performance test: Record by mass, take 1 part of the CSH crystal seed type super early strength agent prepared above, add 35 parts of water and stir evenly, then add 100 parts of standard cement, continue stirring to obtain the cement material modified by CSH crystal seed type super early strength agent. The test indicators of the cement material modified by CSH crystal seed type super early strength agent are: initial setting time is 26min, final setting time is 65min, 6h compressive strength is 12MPa, and 1d compressive strength is 26MPa.

[0038] Example 2

[0039] A CSH seed crystal type super early strength agent, the specific preparation method is as follows:

[0040] (1) 111.66 g of silicon acetate was dissolved in 600 g of tap water, and the mixture was stirred for 50 seconds to obtain a silicon acetate solution. 9.988 g of polycarboxylate was added as a dispersant, and the mixture was stirred to obtain a uniform mixture. The mixture was heated to 85° C. within 7 minutes, and magnetic stirring was performed at a speed of 1500 r / min. A microwave reaction was performed at a microwave power of 600 W for 60 seconds to obtain a reaction intermediate solution I.

[0041] (2) 33.2952 g of calcium sulfate was dissolved in 300 g of tap water, and the mixture was stirred for 50 s to obtain a calcium sulfate solution, which was then added dropwise to the three-necked flask containing the reaction intermediate solution I through a funnel at a rate of 0.1 ml / s. The reaction time was 30 min, and then the mixture was kept warm and cooled for 30 min to obtain a reaction intermediate solution II.

[0042] (3) Add 1% by mass of acrylic acid to the reaction intermediate solution II, stir for 45 seconds to make it evenly mixed, stir for 45 seconds to make it evenly mixed, and then place it in a microwave solid-liquid phase synthesizer, heat it to 85° C. and stir it at a speed of 1200 r / min, react for 10 minutes at a microwave power of 600 W, cool it down and take it out to obtain a seed-type super early strength agent with CSH as the main component.

[0043] Performance test: by mass, take 1 part of the CSH crystal seed type super early strength agent prepared above, add 70 parts of water, stir evenly, add 200 parts of standard cement, continue to stir and shape to obtain the cement material modified by the CSH crystal seed type super early strength agent. The test indicators of the cement material modified by the CSH crystal seed type super early strength agent are: initial setting time is 205min, final setting time is 243min, 6h compressive strength is 11.3MPa, and 1d compressive strength is 24.5MPa.

[0044] In summary, the present invention discloses a CSH seed crystal type super early strength agent, which includes a siliceous raw material, a calcareous raw material, a dispersant, and an organic complexing activator, and has the advantages of effectively shortening the setting time of concrete and developing early strength quickly. The present invention also discloses a preparation method of a CSH seed crystal type super early strength agent, which is mainly prepared by microwave synthesis, and the production process is environmentally friendly and efficient, and meets the requirements of green and sustainable development. The preparation method of the present invention can achieve rapid reaction of raw materials in a short time through microwave heating, and prepare a concrete additive with excellent performance, thereby improving the construction efficiency and quality of construction projects, and has good application prospects in finished concrete, cast-in-place concrete, and mortar. In addition, the preparation method of the present invention also has the characteristics of simple synthesis, short time and high efficiency.

[0045] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the purpose and scope of the technical solution, which should be included in the scope of the claims of the present invention.

Claims

1. A method for preparing a CSH seed crystal type super early strength agent, characterized in that: The preparation method comprises the following steps: (1) adding an aqueous solution of a dispersant having a mass fraction of 10.0% to 30% to a siliceous raw material solution in a three-necked flask in a microwave solid-liquid phase synthesizer, stirring to uniformly mix, and then subjecting to microwave reaction to obtain a reaction intermediate solution I; (2) adding the calcium raw material solution to a three-necked flask to react, and keeping the temperature for 30 to 90 minutes after the reaction to obtain a reaction intermediate solution II; (3) adding an aqueous solution of an organic complexing activator with a mass fraction of 1% to 2% to the reaction intermediate solution II, stirring the mixture to react uniformly, and then transferring the mixture to a microwave solid-liquid phase synthesizer to continue the microwave reaction. After cooling, the mixture is taken out to obtain a CSH seed crystal type super early strength agent.

2. The preparation method according to claim 1, characterized in that In step (1), the mass ratio of the siliceous raw material to water in the siliceous raw material solution is 1:5-20; In step (2), the mass ratio of the calcium raw material to water in the calcium raw material solution is 1:5-20.

3. The preparation method according to claim 1, characterized in that In step (2), the calcium raw material solution is added through a funnel or a syringe pump.

4. The preparation method according to claim 1, characterized in that In step (1), the stirring speed is 1000 r / min to 1500 r / min, and the microwave reaction conditions are: heating to 40° C. to 85° C. within 5 to 10 minutes, and then performing microwave reaction at a power of 400 W to 800 W and a speed of 1000 r / min to 1500 r / min for 30 to 90 seconds; In step (2), the stirring speed is 1000 r / min to 1500 r / min, the dropping speed is 0.1 ml / s to 0.5 ml / s, and the reaction time is 10 to 60 min; In step (3), the microwave reaction conditions are: after heating to 80°C to 95°C, react at a power of 600W to 800W and a rotation speed of 1000r / min to 1500 / min for 30 to 60s.

5. The CSH seed crystal type super early strength agent prepared according to the preparation method according to any one of claims 1 to 4.

6. The CSH seed crystal type super early strength agent according to claim 5, characterized in that: The super early strength agent includes siliceous raw materials, calcium raw materials, dispersants, and organic complexing activators; The molar ratio of the siliceous raw material, the calcareous raw material, the dispersant and the organic complexing activator is 0.8-1.7:1:0.1-0.5:0.01-0.

05.

7. The CSH seed crystal type super early strength agent according to claim 6, characterized in that The siliceous raw material includes any one or more of sodium silicate, silicon acetate, ethyl orthosilicate or silica fume.

8. The CSH seed crystal type super early strength agent according to claim 6, characterized in that The calcium raw material includes any one or more of calcium nitrate, calcium chloride, calcium sulfate or calcium hydroxide.

9. The CSH seed crystal type super early strength agent according to claim 6, characterized in that The dispersant includes any one or more of polycarboxylate ethers, polycarboxylates, or polycarboxylic acid-polyether copolymers; The organic complexing activator includes any one or more of acrylamide, acrylic acid, maleic anhydride, vinyl pyridine, vinyl sulfonic acid or sodium styrene sulfonate.

10. Use of the CSH seed crystal type super early strength agent according to any one of claims 6 to 9 in finished concrete, cast-in-place concrete and mortar.

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