CN112679142B - High-strength epoxy mortar and preparation method thereof - Google Patents
High-strength epoxy mortar and preparation method thereof Download PDFInfo
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Abstract
The application relates to the field of epoxy mortar, and particularly discloses high-strength epoxy mortar and a preparation method thereof. The epoxy mortar comprises a component A and a component B, wherein the component A is prepared from the following raw materials in percentage by weight: 50-80% of epoxy resin, 5-20% of epoxy diluent, 2-10% of thixotropic agent and 8-30% of filler; the component B is prepared from the following raw materials in percentage by weight: 45-75% of a medium-temperature epoxy resin curing agent, 25-55% of carbon nanodots and carbon nanodots for absorbing near infrared light; the weight ratio of the component A to the component B is (1-1.3) to 1; the preparation method comprises the following steps: firstly, dispersing epoxy resin and an epoxy diluent, then adding a thixotropic agent, and finally adding a filler to prepare A; adding the medium-temperature epoxy resin curing agent and the carbon nanodots, and uniformly stirring to obtain B. The method is simple to operate, and the carbon nanodots are uniformly dispersed in the epoxy mortar.
Description
Technical Field
The application relates to the technical field of epoxy mortar, in particular to high-strength epoxy mortar and a preparation method thereof.
Background
Concrete buildings are required to have designed strength while having durability, i.e., skid resistance, abrasion resistance, water resistance, corrosion resistance, and the like. However, many concrete buildings of the prior art have the following problems: 1. concrete building carbonization and crack problems are common; 2. the corrosion of the steel bars caused by the corrosion of the reinforced concrete structure is serious; 3. the surface of the concrete facing water is loosened and peeled off, and the like.
Currently, epoxy mortar is commonly used to improve the above problems. Epoxy mortar is a concrete surface repairing material, and is an epoxy composite material prepared by taking epoxy resin as a main component and adding some auxiliary materials. The epoxy mortar has the characteristics of high strength, good abrasion resistance, strong bonding force, good water resistance and the like; the traditional epoxy mortar is generally used together with an epoxy resin curing agent.
With respect to the related art in the above, the inventors consider that: after the epoxy resin curing agent is added into the epoxy mortar, the epoxy mortar can be cured quickly, so that the construction time of workers is short, and the epoxy mortar is not beneficial to field construction.
Disclosure of Invention
In order to facilitate the construction of the curing rate of the epoxy mortar, the application provides the high-strength epoxy mortar and the preparation method thereof.
The application provides a high-strength epoxy mortar and a preparation method thereof, and the following technical scheme is adopted: the high-strength epoxy mortar comprises a component A and a component B, wherein the component A is prepared from the following raw materials in percentage by weight: 50-80% of epoxy resin, 5-20% of epoxy diluent, 2-10% of thixotropic agent and 8-30% of filler; the component B is prepared from the following raw materials in percentage by weight: 45-75% of a medium-temperature epoxy resin curing agent and 25-55% of carbon nanodots, wherein the carbon nanodots are selected as carbon nanodots for absorbing near infrared light; the weight ratio of the component A to the component B is (1-1.3): 1.
By adopting the technical scheme, the epoxy mortar is slowly cured at normal temperature and mainly exists in the form of cement paste; when the epoxy mortar is irradiated by near infrared light, the carbon nanodots can convert the near infrared light into heat, so that the temperature in an epoxy mortar system is increased; when the temperature is raised to the curing temperature of the medium-temperature epoxy resin curing agent, the medium-temperature epoxy resin curing agent acts on the epoxy resin to promote the epoxy resin to be cured quickly; the carbon nanodots and the medium-temperature epoxy resin curing agent are matched, so that the curing process of the epoxy mortar is controllable, the construction time of a constructor is sufficient, and the construction difficulty is reduced.
Preferably, the component A is prepared from the following raw materials in percentage by weight: 60-70% of epoxy resin, 10-15% of epoxy diluent, 3-7% of thixotropic agent and 12-22% of filler; the component B is prepared from the following raw materials in percentage by weight: 55-65% of medium-temperature epoxy resin curing agent and 35-45% of carbon nanodots, wherein the carbon nanodots are selected from carbon nanodots for absorbing near infrared light, and the weight ratio of the component A to the component B is (1-1.3): 1.
By adopting the technical scheme, the proportion of the epoxy mortar is optimized, the constructor is ensured to have sufficient time for construction, and meanwhile, the epoxy mortar can be ensured to have higher structural strength.
Preferably, the weight ratio of the A component to the B component is 1.18: 1.
By adopting the technical scheme, when the weight ratio of the component A to the component B is adopted, the cured epoxy mortar has higher structural strength.
Preferably, the medium-temperature epoxy mortar curing agent is imidazole epoxy resin curing agent or polyamide curing agent.
By adopting the technical scheme, the polyamide curing agent and the imidazole epoxy resin curing agent can efficiently promote the curing of the epoxy resin; compared with imidazole epoxy resin curing agents, the polyamide curing agent has certain adhesiveness, is beneficial to solid-phase adhesion and aggregation in concrete, and plays a role in enhancing the early strength of the concrete.
Preferably, the carbon nanodots are amino POSS modified carbon nanodots.
By adopting the technical scheme, the amino POSS is rich in amino, can perform amidation reaction with carboxyl on the surface of the carbon nanodot, and is easy to graft the amino POSS on the carbon nanodot;
the silicon-oxygen framework formed by alternately connecting Si-O of the amino POSS enables the carbon nanodots to absorb near infrared light with higher frequency, and the photo-thermal conversion efficiency of the carbon nanodots is further improved; in addition, amino POSS can be filled in epoxy resin, so that the strength of the cured epoxy mortar is further improved.
Preferably, the preparation method of the amino POSS modified carbon nanodots comprises the following steps:
activation of the carbon nanodots: weighing carbon nanodots, and putting the carbon nanodots into tetrahydrofuran to prepare a dispersion liquid; heating the dispersion liquid at a constant temperature of 50-70 ℃, adding N, N-carbonyldiimidazole into the dispersion liquid according to the weight ratio of the carbon nanodots to the N, N-carbonyldiimidazole being (8-12): 1, stirring and activating to obtain activated carbon nanodots;
modified amino POSS: the weight ratio of the amino POSS to the carbon nanodots is (0.3-0.6): 1, adding amino POSS into tetrahydrofuran, and performing dispersion treatment to obtain POSS dispersion liquid. Mixing the amino POSS dispersion liquid with the activated carbon nanodots, and stirring and reacting at 50-70 ℃ for 12-18 h; and filtering and drying to obtain the amino POSS modified carbon nanodots.
By adopting the technical scheme, the carboxyl on the carbon nanodots is activated by using N, N-carbonyl diimidazole, and then the amino POSS is mixed with the activated carbon nanodots, so that the amino of the amino POSS and the carboxyl of the activated carbon nanodots are subjected to amidation reaction, and the amino POSS modified carbon nanodots can be obtained after treatment.
Preferably, the thixotropic agent is oleophilic modified fumed silica.
By adopting the technical scheme, the oleophylic modified gas-phase silica has the advantages of small particle size, more micropores, large specific surface area and the like, and the oleophylic modified gas-phase silica has high surface hydroxyl content and strong ultraviolet, visible light and infrared reflection capability, can reflect light rays into the carbon nanodots, and further improves the near infrared light absorbed by the carbon nanodots;
meanwhile, the oleophylic modified fumed silica has fewer silicon hydroxyl groups on the surface and better self hydrophobicity, and the stability and the dispersibility of the thixotropic agent in the epoxy resin are prolonged, so that the near infrared light absorption efficiency of the carbon nanodots is improved.
Preferably, the epoxy diluent is one of ethylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether and benzyl glycidyl ether.
By adopting the technical scheme, the ethylene glycol diglycidyl ether, the polypropylene glycol diglycidyl ether and the benzyl glycidyl ether are reactive diluents, and the structural strength of the epoxy mortar can be increased after the reaction.
Preferably, the filler is heavy calcium carbonate and mica flakes in a weight ratio of (1-3): 1, compounding.
By adopting the technical scheme, after the epoxy resin is cured, the crack propagation resistance is poor, the epoxy resin is a brittle material, and the heavy calcium carbonate is irregular and granular, so that the epoxy mortar is easier to generate stress concentration and crack deflection when being damaged by stress; the mica flake has a flat lamellar structure and a large flake diameter, can prevent the crack propagation of epoxy mortar when the epoxy mortar is damaged by stress, and is beneficial to improving the structural strength of the epoxy mortar by compounding the mica flake and the epoxy mortar.
In a second aspect, the present application provides a method for preparing a high-strength epoxy mortar, which adopts the following technical scheme:
a preparation method of high-strength epoxy mortar comprises the following steps:
mixing the component A: firstly, dispersing epoxy resin and an epoxy diluent, adding a thixotropic agent after uniform dispersion, dispersing, adding a filler, and uniformly dispersing for later use;
mixing the component B: and (3) sequentially adding the medium-temperature epoxy resin curing agent and the carbon nanodots in parts by weight, and uniformly stirring for later use.
By adopting the technical scheme, the component A and the component B are respectively prepared according to the weight parts of the components, and are separately stored, namely the components are prepared and used, and the site construction is convenient.
In summary, the present application has the following beneficial effects:
1. as the carbon nanodots and the medium-temperature epoxy resin curing agent are matched for use, the epoxy mortar can be rapidly cured, the strength of the epoxy mortar can be improved, and the effect is excellent.
2. In the application, the carbon nanodots are modified by the amino POSS, so that near-infrared absorption performance of the carbon nanodots is improved, and photo-thermal conversion efficiency of the carbon nanotubes is also improved; the amino POSS modified carbon nanodots can be used as a framework to be filled in epoxy resin, so that the strength of a cured epoxy mortar is further improved.
3. According to the application, oleophylic modified fumed silica is used as a thixotropic agent, so that the storage stability of the epoxy resin is enhanced, the high dispersibility is realized, the structuring phenomenon is eliminated, and the tensile strength of the epoxy resin is improved.
4. The compound of the heavy calcium carbonate and the mica flakes is selected as the filler of the epoxy mortar, so that the strength of the epoxy mortar is further improved.
Detailed Description
The present application will be described in further detail with reference to examples.
The raw materials used in the examples of the present application are commercially available, wherein the epoxy resin is obtained from Hubei Fujiali building materials science and technology Co., Ltd, the polypropylene glycol diglycidyl ether is obtained from Australian Industrial development (Shanghai) Co., Ltd, the type of the oleophilic modified fumed silica is VK-SP30S, and the carbon nanodots are prepared according to the preparation method disclosed in example 3 of the invention patent with the publication number CN 104495782B.
Preparation examples of raw materials
Preparing amino POSS modified carbon nanodots:
activation of the carbon nanodots: weighing 2kg of carbon nanodot powder, placing the carbon nanodot powder in a beaker, adding 0.5L of tetrahydrofuran, and placing the mixture in an ultrasonic machine for ultrasonic dispersion for 3 hours to obtain a mixture 1; pouring the mixture 1 into a four-mouth bottle, performing constant-temperature water bath at 60 ℃ in a water bath kettle, adding 0.24kg of N, N-carbonyldiimidazole for activation, and stirring and activating for 4 hours under the condition that the temperature of the water bath is maintained at 60 ℃ to obtain activated carbon nanodots;
modified amino POSS: weighing 1kg of amino POSS in a three-necked flask, adding 0.6L of tetrahydrofuran, and performing ultrasonic dispersion for 2 hours to obtain a well-dispersed amino POSS solution. Adding amino POSS solution into a four-mouth bottle containing activated carbon nanodots, stirring at 60 ℃ for reaction for 15h, and continuously introducing N in the reaction process2. After the reaction is finished, carrying out suction filtration for 15min, and placing a solid sample obtained after suction filtration at 80 ℃ for vacuum drying for 72 h. After drying, the dried solid sample was ground with a mortar to obtain amino POSS modified carbon nanodots.
Examples
Examples 1 to 5
As shown in Table 1, examples 1 to 5 are different in the ratio of raw materials.
The following description will be given by taking example 1 as an example.
The epoxy mortar provided in example 1 was prepared as follows:
s1, weighing a component A and a component B according to a formula ratio;
s2, mixing the component A: firstly, uniformly dispersing epoxy resin and an epoxy diluent at 50r/min, grinding until the fineness is less than or equal to 80 mu m, adding a thixotropic agent, dispersing at 50r/min for 10min, then dispersing at 250r/min for 2-3 min, finally adding a filler, uniformly dispersing, and packaging;
and S3, mixing the components B: weighing the medium-temperature epoxy resin curing agent and the carbon nanodots in sequence according to the formula proportion, mixing, stirring for 1h at the speed of 50r/min, and filtering;
and S4, mixing the component A and the component B at the speed of 50r/min for 1h to obtain the epoxy mortar.
Wherein, the thixotropic agent adopts fumed silica, the filler adopts heavy calcium carbonate, the epoxy diluent adopts ethylene glycol diglycidyl ether, the medium-temperature epoxy resin curing agent adopts imidazole epoxy resin curing agent, and the imidazole epoxy resin curing agent is purchased from complex new materials (Shanghai) Limited company.
TABLE 1
Example 6
This example differs from example 3 in that the epoxy diluent is polypropylene glycol diglycidyl ether.
Example 7
This example differs from example 3 in that benzyl glycidyl ether was used as the epoxy diluent.
Example 8
This example differs from example 7 in that the thixotropic agent is an oleophilic modified fumed silica.
Example 9
The difference between the embodiment and the embodiment 8 is that the filler is heavy calcium carbonate and mica flake in a weight ratio of 1: 1, compounding.
Example 10
The difference between the embodiment and the embodiment 8 is that the filler is heavy calcium carbonate and mica flake in a weight ratio of 2: 1, compounding.
Example 11
The difference between the embodiment and the embodiment 8 is that the filler is heavy calcium carbonate and mica flake in a weight ratio of 3: 1, compounding.
Example 12
This example is different from example 10 in that a polyether amine curing agent 651 is used as the curing agent.
Example 13
The difference between this example and example 12 is that the amino POSS modified carbon nanodots prepared in the preparation example were used as the carbon nanodots.
Comparative example
Comparative example 1
The epoxy mortar is prepared according to the preparation method disclosed in the embodiment 4 of the Chinese patent with the publication number of CN 103359977B.
Comparative example 2
Compared with the example 3, the normal-temperature epoxy resin curing agent is used for replacing the medium-temperature epoxy resin curing agent in the formula, and the normal-temperature epoxy resin curing agent is polythiol which is purchased from a new complexing material (Shanghai) company Limited.
Comparative example 3
In comparison with example 3, the intermediate temperature epoxy resin curing agent in the formulation was replaced with a high temperature epoxy resin curing agent selected from boc acetic anhydride, which was obtained from Baishun (Beijing) chemical technology, Inc.
Performance test
Preparing epoxy mortar and test blocks:
(1) storing the materials for the test at (23 +/-2) DEG C for at least 24 h;
(2) mixing materials: respectively stirring the weighed liquid and the filler uniformly, pouring the mixture into a stirring pot in sequence, starting a stirrer to slowly and uniformly stir until the color is uniform and no caking exists in the mixture;
(3) block making: filling the stirred mortar into a test mold, filling for 2 times, and compacting by using a pounding knife or a pounding rod every time, wherein the top of the mortar is slightly higher than the upper surface of the test mold; finally, scraping the raised materials to be flush with the surface of the test mold, numbering the test mold, irradiating the test mold by using near infrared light, and recording the operable time and the initial setting time; when the mixture is not free flowing, the mortar filler can be extruded into the test mould by a compacting tool to make it be filled tightly without holes. After the test piece is molded, the test piece is put into air with the temperature of (23 +/-2) DEG C and the relative humidity of (50 +/-5)% for curing for 28 d.
The compressive strength, tensile strength, curing time, etc. of the epoxy mortar were tested with reference to DL/T5193-2004 technical Specification for epoxy mortar.
The compressive strength, tensile strength, bond strength and flexural strength to concrete, initial setting time and working time were measured for examples 1 to 13 and comparative examples 1 to 3, and the data are shown in table 2 below.
Detection method
TABLE 2
By combining the examples 1-8 and the comparative example 1, after the medium-temperature epoxy resin curing agent, the carbon nanodots and the epoxy resin are mixed, the performances of tensile strength, breaking strength, compressive strength and the like of the cured epoxy mortar can be effectively improved, and the operable time is particularly increased, because the medium-temperature epoxy resin curing agent and the epoxy resin are cured slowly at normal temperature, sufficient construction time is reserved for constructors; when the epoxy mortar is illuminated by near infrared light, the carbon nanodots can absorb the near infrared light and convert the light energy into heat energy, so that the temperature of the epoxy mortar system reaches the optimal curing temperature of the curing agent to achieve the effect of rapid curing, and when the weight ratio of the component A to the component B is 1.18:1, the obtained epoxy mortar has better tensile strength, folding strength and compressive strength.
With reference to examples 1 to 8, it can be seen that when the weight ratio of the carbon nanodots to the medium-temperature epoxy resin curing agent is 2:3, the tensile strength, the flexural strength and the compressive strength of the obtained epoxy mortar cured product are optimal, and when the weight content of the medium-temperature epoxy resin curing agent is reduced, the operable time and the initial setting time of the epoxy mortar are prolonged, and the tensile strength, the flexural strength and the compressive strength after curing are reduced; when the content of the carbon nanodots is increased, the operable time and the initial setting time of the epoxy mortar are reduced, and the tensile strength, the flexural strength and the compressive strength after curing are reduced.
By combining the embodiment 3 and the comparative examples 2 to 3, the epoxy resin has more excellent tensile strength, breaking strength, compressive strength and operability time under the action of the medium-temperature epoxy resin curing agent, and the operability time is too short because the epoxy resin can be cured at normal temperature due to too low curing temperature of the normal-temperature epoxy resin curing agent; after the carbon nano-dots absorb near infrared rays, the emitted heat cannot reach the curing heat of the high-temperature epoxy resin curing agent easily, so that the high-temperature epoxy resin curing agent cannot be matched with the carbon nano-dots to promote the curing of the epoxy resin.
By combining the embodiment 12 and the embodiment 13, the amino POSS modified carbon nanodots have higher photo-thermal conversion rate, because after the amino group on the amino POSS is grafted with the carbon nanodots, the cage-type framework of the amino POSS improves the optical properties of the carbon nanodots, and meanwhile, the amino POSS nanoparticles can initiate the rearrangement of the molecular chains of the carbon nanodots, thereby significantly enhancing the strength of the epoxy mortar.
By combining the embodiment 7 and the embodiment 8, the thixotropic agent adopts oleophylic modified fumed silica, which has stronger visible light and infrared ray reflection capability, reflects light rays into the carbon nanodots, further increases the near infrared ray absorption amount of the carbon nanodots, and simultaneously, the oleophylic modified fumed silica can improve the tensile property of the epoxy mortar and can further improve the tensile strength, the breaking strength and the compressive strength of the cured epoxy mortar.
By combining examples 9-11 and 8, when the filler is compounded by heavy calcium carbonate and mica flakes, the strength and compression resistance of the epoxy mortar cured material are effectively improved, because the mica flakes have a flat lamellar structure, when the epoxy mortar is damaged by stress, the crack propagation of the epoxy mortar cured material can be prevented; and the heavy calcium carbonate is irregular particles, so that stress concentration and crack deflection easily occur when the epoxy mortar is damaged by stress, and the mica flakes and the heavy calcium carbonate are compounded, which is beneficial to improving the tensile strength, the breaking strength and the compressive strength of the cured epoxy mortar.
When the polyamide curing agent is selected as the medium-temperature epoxy resin curing agent, the bonding strength between the cured epoxy resin and the concrete is higher by combining the embodiment 10 and the embodiment 12, because the polyamide curing agent can cure the epoxy resin, has good self-bonding performance and greatly increases the early strength of the concrete.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. The high-strength epoxy mortar is characterized by comprising a component A and a component B, wherein the component A is prepared from the following raw materials in percentage by weight: 50-80% of epoxy resin, 5-20% of epoxy diluent, 2-10% of thixotropic agent and 8-30% of filler; the component B is prepared from the following raw materials in percentage by weight: 45-75% of a medium-temperature epoxy resin curing agent and 25-55% of carbon nanodots, wherein the carbon nanodots are selected as carbon nanodots for absorbing near infrared light; the weight ratio of the component A to the component B is (1-1.3) to 1;
the carbon nanodots are amino POSS modified carbon nanodots;
the preparation method of the amino POSS modified carbon nanodot comprises the following steps:
activation of the carbon nanodots: weighing carbon nanodots, and dissolving the carbon nanodots in tetrahydrofuran to prepare a dispersion liquid; heating the dispersion liquid at a constant temperature of 50-70 ℃, adding N, N-carbonyldiimidazole into the dispersion liquid according to the weight ratio of the carbon nanodots to the N, N-carbonyldiimidazole being (8-12): 1, stirring and activating to obtain activated carbon nanodots;
modified amino POSS: the weight ratio of the amino POSS to the carbon nanodots is (0.3-0.6): 1, adding amino POSS into tetrahydrofuran, and performing dispersion treatment to obtain POSS dispersion liquid;
mixing the POSS dispersion liquid with the activated carbon nanodots, and stirring and reacting at 50-70 ℃ for 12-18 h; and filtering and drying to obtain the amino POSS modified carbon nanodots.
2. The high-strength epoxy mortar according to claim 1, wherein: the component A is prepared from the following raw materials in percentage by weight: 60-70% of epoxy resin, 10-15% of epoxy diluent, 3-7% of thixotropic agent and 12-22% of filler; the component B is prepared from the following raw materials in percentage by weight: 55-65% of medium-temperature epoxy resin curing agent and 35-45% of carbon nanodots, wherein the carbon nanodots are selected from carbon nanodots for absorbing near infrared light, and the weight ratio of the component A to the component B is (1-1.3): 1.
3. The high-strength epoxy mortar according to claim 1, wherein: the weight ratio of the component A to the component B is 1.18: 1.
4. The high-strength epoxy mortar according to claim 1, wherein: the medium-temperature epoxy mortar curing agent is imidazole epoxy resin curing agent or polyamide curing agent.
5. The high-strength epoxy mortar according to claim 1, wherein: the thixotropic agent is oleophylic modified fumed silica.
6. The high-strength epoxy mortar according to claim 1, wherein: the epoxy diluent is one of ethylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether and benzyl glycidyl ether.
7. The high-strength epoxy mortar according to claim 1, wherein: the filler is prepared from heavy calcium carbonate and mica flakes according to the weight ratio of (1-3): 1, compounding.
8. The preparation method of the high-strength epoxy mortar according to any one of claims 1 to 7, characterized by comprising the following steps:
mixing the component A: firstly, dispersing epoxy resin and an epoxy diluent, adding a thixotropic agent after uniform dispersion, fully dispersing, adding a filler, and uniformly dispersing for later use;
mixing the component B: and (3) sequentially adding the medium-temperature epoxy resin curing agent and the carbon nanodots in parts by weight, and uniformly stirring for later use.
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