CN111073219A - Preparation method of high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction - Google Patents
Preparation method of high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention relates to a preparation method of high-strength anti-yellowing anti-freezing and thawing resistant epoxy resin for sponge city construction, which comprises the steps of preparation of an epoxy resin main agent, preparation of a functionalized carbon nano tube, preparation of a reinforcing and toughening solution, preparation of a curing agent and preparation of the epoxy resin. The epoxy resin casting body prepared by the method has the advantages of high strength, good toughness, small shrinkage rate and good freeze-thaw resistance.
Description
Technical Field
The invention belongs to the technical field of novel epoxy resin, and particularly relates to a preparation method of high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction.
Background
The sponge city is a city development mode which fully exerts the functions of absorption, storage and seepage and slow release of rainwater by building, road, greenbelt, water system and other ecological systems by strengthening city planning construction management, effectively controls rainwater runoff, and realizes natural accumulation, natural seepage and natural purification. Sponge city construction follows principles such as ecological priority, combines natural approach and artificial technology, and under the prerequisite of guaranteeing urban drainage waterlogging prevention safety, furthest realizes that rainwater accumulates in urban area, infiltration and purifies, promotes the utilization of rainwater resource and ecological environment protection.
The construction of sponge cities requires the use of water permeable bricks and water permeable ground, the water permeable bricks and the water permeable ground need to be bonded with epoxy resin, and the conventional epoxy resin cannot meet the use requirements due to the compression strength and the freeze-thaw resistance.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of high-strength anti-yellowing anti-freezing and thawing resistant epoxy resin for sponge city construction, which comprises the following steps in sequence:
(1) adding 4, 4' -diaminodiphenylmethane tetraglycidyl amine, bisphenol F epoxy resin, trimethylolpropane triglycidyl ether and a low-temperature epoxy resin reinforcing agent into a reaction kettle, and stirring to obtain an epoxy resin main agent, wherein the low-temperature epoxy resin reinforcing agent is aromatic polyester;
(2) adding carbon nano tubes and a coupling agent into deionized water, uniformly stirring to obtain a mixture, dispersing the mixture by a dispersion machine to obtain a solution in which the carbon nano tubes are dispersed, cleaning the dispersed carbon nano tubes by ethanol or acetone, and drying the cleaned carbon nano tubes to obtain the functionalized carbon nano tubes, wherein the coupling agent is a silane coupling agent containing epoxy functional groups;
(3) filling trimethylolpropane triglycidyl ether, the functionalized carbon nano tube prepared in the second step and benzyl alcohol into a reaction kettle, fully stirring the materials in the reaction kettle, and fully and uniformly dispersing the functionalized carbon nano tube in the matching reinforcing and toughening liquid through ultrahigh frequency oscillation to prepare the matching reinforcing and toughening liquid;
(4) mixing 95 parts of modified alicyclic amine epoxy curing agent IPDA-isophorone diamine and 5 parts of modified curing accelerator LMC to prepare a curing agent;
(5) and (3) stirring and combining the epoxy resin main agent prepared in the step (1), the matching reinforcing and toughening liquid prepared in the step (3) and the curing agent prepared in the step (4) to obtain the high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction.
Preferably, the detailed steps of step (1) are: weighing 60-75 parts of 4, 4' -diaminodiphenylmethane tetraglycidyl amine, 30-40 parts of bisphenol F epoxy resin, 5-10 parts of trimethylolpropane triglycidyl ether and 5 parts of self-made low-temperature epoxy resin reinforcing agent, filling into a reaction kettle, and vacuumizing and stirring at the temperature of 40-60 ℃ for 90 minutes to obtain the epoxy resin main agent.
In any of the above schemes, the detailed steps of step (2) are preferably: adding 1-6 parts by weight of carbon nano tube and 8-11 parts by weight of coupling agent into 100 parts by weight of deionized water, and fully and uniformly stirring at 25-40 ℃ to obtain a mixture, wherein the diameter of the carbon nano tube is 0.5-50 nm, the length of the carbon nano tube is 2-30 microns, the coupling agent is a silane coupling agent containing epoxy functional groups, highly dispersing the mixture at 80 ℃ by a dispersion machine to obtain a solution in which the carbon nano tube is dispersed, cleaning the dispersed carbon nano tube by using ethanol or acetone, and drying the cleaned carbon nano tube at 80-100 ℃ for 180 minutes to obtain the functionalized carbon nano tube.
In any of the above schemes, the detailed steps of step (3) are preferably: weighing 80-90 parts by weight of trimethylolpropane triglycidyl ether, 3-10 parts by weight of the functionalized carbon nano tube prepared in the second step and 10-20 parts by weight of benzyl alcohol, filling the materials into a reaction kettle, fully stirring the materials at the temperature of 25-45 ℃, and fully and uniformly dispersing the functionalized carbon nano tube in the matching reinforcing and toughening liquid through ultrahigh frequency oscillation to finally prepare the matching reinforcing and toughening liquid.
In any of the above schemes, preferably, in step (5), the amounts of the respective ingredients added are: 100 parts of epoxy resin main agent is added with 40-50 parts of curing agent and 8-20 parts of matching reinforcing toughening liquid.
In any of the above embodiments, it is preferable that the stirring temperature in the step (5) is: 25-45 ℃.
The invention has the beneficial effects that: the epoxy resin casting body prepared by the method has the advantages of high strength, good toughness, small shrinkage rate and good freeze-thaw resistance.
Detailed Description
In order that the invention may be further understood, the invention will now be described in detail with reference to specific examples.
Example one
A preparation method of high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction comprises the following steps in sequence:
(1) weighing 60 parts of 4, 4' -diaminodiphenylmethane tetraglycidyl amine, 30 parts of bisphenol F epoxy resin, 5 parts of trimethylolpropane triglycidyl ether and 5 parts of self-made low-temperature epoxy resin reinforcing agent, filling the materials into a reaction kettle, and vacuumizing and stirring the materials at the temperature of 40 ℃ for 90 minutes to obtain an epoxy resin main agent;
(2) adding 1 part by weight of carbon nano tube and 8 parts by weight of coupling agent into 100 parts by weight of deionized water, and fully and uniformly stirring at 25 ℃ to obtain a mixture, wherein the diameter of the carbon nano tube is 0.5-50 nm, the length of the carbon nano tube is 2-30 microns, the coupling agent is a silane coupling agent containing epoxy functional groups, the mixture is highly dispersed at 80 ℃ by a dispersion machine to obtain a solution with dispersed carbon nano tubes, the dispersed carbon nano tubes are cleaned by ethanol or acetone, and the cleaned carbon nano tubes are dried at 80 ℃ for 180 minutes to obtain functionalized carbon nano tubes;
(3) weighing 80 parts by weight of trimethylolpropane triglycidyl ether, 3 parts by weight of the functionalized carbon nano tube prepared in the second step and 10 parts by weight of benzyl alcohol, filling the materials into a reaction kettle, fully stirring the materials at the temperature of 25 ℃, and fully and uniformly dispersing the functionalized carbon nano tube in the matching reinforcing and toughening liquid through ultrahigh frequency oscillation to finally prepare the matching reinforcing and toughening liquid;
(4) mixing 95 parts of modified alicyclic amine epoxy curing agent IPDA-isophorone diamine and 5 parts of modified curing accelerator LMC to prepare a curing agent;
(5) and adding 40 parts by weight of curing agent and 8 parts by weight of matching reinforcing and toughening liquid into 100 parts of epoxy resin main agent, and stirring and combining at the temperature of 25 ℃ to obtain the high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction.
Example two
A preparation method of high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction comprises the following steps in sequence:
(1) weighing 65 parts of 4, 4' -diaminodiphenylmethane tetraglycidyl amine, 33 parts of bisphenol F epoxy resin, 6 parts of trimethylolpropane triglycidyl ether and 5 parts of self-made low-temperature epoxy resin reinforcing agent, filling into a reaction kettle, and vacuumizing and stirring at the temperature of 50 ℃ for 90 minutes to obtain an epoxy resin main agent;
(2) adding 2 parts by weight of carbon nano tubes and 9 parts by weight of coupling agent into 100 parts by weight of deionized water, and fully and uniformly stirring at the temperature of 30 ℃ to prepare a mixture, wherein the tube diameter of the carbon nano tubes is 0.5-50 nanometers, the length of the carbon nano tubes is 2-30 micrometers, the coupling agent is a silane coupling agent containing epoxy functional groups, the mixture is highly dispersed at the temperature of 80 ℃ by a dispersion machine to prepare a solution in which the carbon nano tubes are dispersed, the dispersed carbon nano tubes are cleaned by ethanol or acetone, and the cleaned carbon nano tubes are dried for 180 minutes at the temperature of 90 ℃ to prepare functionalized carbon nano tubes;
(3) weighing 82 parts by weight of trimethylolpropane triglycidyl ether, 4 parts by weight of the functionalized carbon nano tube prepared in the second step and 12 parts by weight of benzyl alcohol, filling the weighed materials into a reaction kettle, fully stirring the materials at the temperature of 35 ℃, and fully and uniformly dispersing the functionalized carbon nano tube in the matching, reinforcing and toughening liquid through ultrahigh frequency oscillation to finally prepare the matching, reinforcing and toughening liquid;
(4) mixing 95 parts of modified alicyclic amine epoxy curing agent IPDA-isophorone diamine and 5 parts of modified curing accelerator LMC to prepare a curing agent;
(5) and adding 42 parts by weight of curing agent and 11 parts by weight of matching reinforcing and toughening liquid into 100 parts of epoxy resin main agent, and stirring and combining at the temperature of 35 ℃ to obtain the high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction.
EXAMPLE III
A preparation method of high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction comprises the following steps in sequence:
(1) weighing 70 parts of 4, 4' -diaminodiphenylmethane tetraglycidyl amine, 35 parts of bisphenol F epoxy resin, 7 parts of trimethylolpropane triglycidyl ether and 5 parts of self-made low-temperature epoxy resin reinforcing agent, filling into a reaction kettle, and vacuumizing and stirring at the temperature of 55 ℃ for 90 minutes to obtain an epoxy resin main agent;
(2) adding 3 parts by weight of carbon nano tubes and 10 parts by weight of coupling agent into 100 parts by weight of deionized water, and fully and uniformly stirring at 38 ℃ to obtain a mixture, wherein the tube diameter of the carbon nano tubes is 0.5-50 nm, the length of the carbon nano tubes is 2-30 microns, the coupling agent is a silane coupling agent containing epoxy functional groups, the mixture is highly dispersed at 80 ℃ by a dispersion machine to obtain a solution with dispersed carbon nano tubes, the dispersed carbon nano tubes are cleaned by ethanol or acetone, and the cleaned carbon nano tubes are dried at 100 ℃ for 180 minutes to obtain functionalized carbon nano tubes;
(3) weighing 85 parts by weight of trimethylolpropane triglycidyl ether, 7 parts by weight of the functionalized carbon nano tube prepared in the second step and 15 parts by weight of benzyl alcohol, filling the weighed materials into a reaction kettle, fully stirring the materials at the temperature of 40 ℃, and fully and uniformly dispersing the functionalized carbon nano tube in the matching, reinforcing and toughening liquid through ultrahigh frequency oscillation to finally prepare the matching, reinforcing and toughening liquid;
(4) mixing 95 parts of modified alicyclic amine epoxy curing agent IPDA-isophorone diamine and 5 parts of modified curing accelerator LMC to prepare a curing agent;
(5) and adding 45 parts by weight of curing agent and 15 parts by weight of matching reinforcing and toughening liquid into 100 parts of epoxy resin main agent, and stirring and combining at 40 ℃ to obtain the high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction.
Example four
A preparation method of high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction comprises the following steps in sequence:
(1) weighing 70 parts of 4, 4' -diaminodiphenylmethane tetraglycidyl amine, 38 parts of bisphenol F epoxy resin, 9 parts of trimethylolpropane triglycidyl ether and 5 parts of self-made low-temperature epoxy resin reinforcing agent, filling into a reaction kettle, and vacuumizing and stirring at the temperature of 60 ℃ for 90 minutes to obtain an epoxy resin main agent;
(2) adding 5 parts by weight of carbon nano tubes and 10 parts by weight of coupling agent into 100 parts by weight of deionized water, and fully and uniformly stirring at 40 ℃ to obtain a mixture, wherein the tube diameter of the carbon nano tubes is 0.5-50 nanometers, the length of the carbon nano tubes is 2-30 micrometers, the coupling agent is a silane coupling agent containing epoxy functional groups, the mixture is highly dispersed at 80 ℃ by a dispersion machine to obtain a solution with dispersed carbon nano tubes, the dispersed carbon nano tubes are cleaned by ethanol or acetone, and the cleaned carbon nano tubes are dried at 100 ℃ for 180 minutes to obtain functionalized carbon nano tubes;
(3) weighing 88 parts by weight of trimethylolpropane triglycidyl ether, 9 parts by weight of the functionalized carbon nanotube prepared in the second step and 18 parts by weight of benzyl alcohol, filling the materials into a reaction kettle, fully stirring the materials at 42 ℃ and fully and uniformly dispersing the functionalized carbon nanotube in the matching reinforcing and toughening liquid through ultrahigh frequency oscillation, and finally preparing the matching reinforcing and toughening liquid;
(4) mixing 95 parts of modified alicyclic amine epoxy curing agent IPDA-isophorone diamine and 5 parts of modified curing accelerator LMC to prepare a curing agent;
(5) and adding 48 parts by weight of curing agent and 18 parts by weight of matching reinforcing and toughening liquid into 100 parts of epoxy resin main agent, and stirring and combining at the temperature of 45 ℃ to obtain the high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction.
EXAMPLE five
A preparation method of high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction comprises the following steps in sequence:
(1) weighing 75 parts of 4, 4' -diaminodiphenylmethane tetraglycidyl amine, 40 parts of bisphenol F epoxy resin, 10 parts of trimethylolpropane triglycidyl ether and 5 parts of self-made low-temperature epoxy resin reinforcing agent, filling into a reaction kettle, and vacuumizing and stirring at the temperature of 55 ℃ for 90 minutes to obtain an epoxy resin main agent;
(2) adding 6 parts by weight of carbon nano tubes and 11 parts by weight of coupling agent into 100 parts by weight of deionized water, and fully and uniformly stirring at 40 ℃ to obtain a mixture, wherein the tube diameter of the carbon nano tubes is 0.5-50 nanometers, the length of the carbon nano tubes is 2-30 micrometers, the coupling agent is a silane coupling agent containing epoxy functional groups, the mixture is highly dispersed at 80 ℃ by a dispersion machine to obtain a solution with dispersed carbon nano tubes, the dispersed carbon nano tubes are cleaned by ethanol or acetone, and the cleaned carbon nano tubes are dried at 90 ℃ for 180 minutes to obtain functionalized carbon nano tubes;
(3) weighing 90 parts by weight of trimethylolpropane triglycidyl ether, 10 parts by weight of the functionalized carbon nano tube prepared in the second step and 20 parts by weight of benzyl alcohol, filling the weighed materials into a reaction kettle, fully stirring the materials at the temperature of 45 ℃, and fully and uniformly dispersing the functionalized carbon nano tube in the matching, reinforcing and toughening liquid through ultrahigh frequency oscillation to finally prepare the matching, reinforcing and toughening liquid;
(4) mixing 95 parts of modified alicyclic amine epoxy curing agent IPDA-isophorone diamine and 5 parts of modified curing accelerator LMC to prepare a curing agent;
(5) and adding 50 parts by weight of curing agent and 20 parts by weight of matching reinforcing and toughening liquid into 100 parts of epoxy resin main agent, and stirring and combining at 40 ℃ to obtain the high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction.
Performance testing
And (4) carrying out performance tests on the sponge city constructed by the high-strength anti-yellowing anti-freezing epoxy resin prepared in the fifth embodiment and the water permeable brick prepared from stones, wherein the test contents comprise compressive strength and freezing and thawing resistance.
TABLE 1 test results
As shown in Table 1, the epoxy resin prepared by the method of the invention has high temperature resistance and outstanding low temperature resistance, the low temperature performance including compressive strength at minus 45-50 ℃ is high, and the resin casting bodies of other epoxy resins on the market are generally embrittled at minus 30 ℃, while the water permeable brick prepared by the epoxy resin of the invention can be subjected to freeze-thaw cycle at minus 30 ℃ for 75 times, and can meet the production and use requirements of products such as construction of water permeable bricks in sponge cities and integral pavement of water permeable pavements.
It will be understood by those skilled in the art that the preparation method of the high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction according to the present invention includes the summary and the detailed description of the present specification, which are limited to space and not described in the embodiments of the combination for the sake of brevity. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A preparation method of high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction comprises the following steps in sequence:
(1) adding 4, 4' -diaminodiphenylmethane tetraglycidyl amine, bisphenol F epoxy resin, trimethylolpropane triglycidyl ether and a low-temperature epoxy resin reinforcing agent into a reaction kettle, and stirring to obtain an epoxy resin main agent;
(2) adding carbon nano tubes and a coupling agent into deionized water, uniformly stirring to obtain a mixture, dispersing the mixture by a dispersion machine to obtain a solution in which the carbon nano tubes are dispersed, cleaning the dispersed carbon nano tubes by ethanol or acetone, and drying the cleaned carbon nano tubes to obtain the functionalized carbon nano tubes, wherein the coupling agent is a silane coupling agent containing epoxy functional groups;
(3) filling trimethylolpropane triglycidyl ether, the functionalized carbon nano tube prepared in the second step and benzyl alcohol into a reaction kettle, fully stirring the materials in the reaction kettle, and fully and uniformly dispersing the functionalized carbon nano tube in the matching reinforcing and toughening liquid through ultrahigh frequency oscillation to prepare the matching reinforcing and toughening liquid;
(4) mixing 95 parts of modified alicyclic amine epoxy curing agent IPDA-isophorone diamine and 5 parts of modified curing accelerator LMC to prepare a curing agent;
(5) and (3) stirring and combining the epoxy resin main agent prepared in the step (1), the matching reinforcing and toughening liquid prepared in the step (3) and the curing agent prepared in the step (4) to obtain the high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction.
2. The preparation method of the high-strength anti-yellowing freeze-thaw resistant epoxy resin for sponge city construction according to claim 1, wherein the detailed steps of the step (1) are as follows: weighing 60-75 parts of 4, 4' -diaminodiphenylmethane tetraglycidyl amine, 30-40 parts of bisphenol F epoxy resin, 5-10 parts of trimethylolpropane triglycidyl ether and 5 parts of self-made low-temperature epoxy resin reinforcing agent, filling into a reaction kettle, and vacuumizing and stirring at the temperature of 40-60 ℃ for 90 minutes to obtain the epoxy resin main agent.
3. The preparation method of the high-strength anti-yellowing freeze-thaw resistant epoxy resin for sponge city construction according to claim 1, wherein the detailed step of the step (2) is: adding 1-6 parts by weight of carbon nano tube and 8-11 parts by weight of coupling agent into 100 parts by weight of deionized water, and fully and uniformly stirring at 25-40 ℃ to obtain a mixture, wherein the diameter of the carbon nano tube is 0.5-50 nm, the length of the carbon nano tube is 2-30 microns, the coupling agent is a silane coupling agent containing epoxy functional groups, highly dispersing the mixture at 80 ℃ by a dispersion machine to obtain a solution in which the carbon nano tube is dispersed, cleaning the dispersed carbon nano tube by using ethanol or acetone, and drying the cleaned carbon nano tube at 80-100 ℃ for 180 minutes to obtain the functionalized carbon nano tube.
4. The preparation method of the high-strength anti-yellowing freeze-thaw resistant epoxy resin for sponge city construction according to claim 1, wherein the detailed step of the step (3) is: weighing 80-90 parts by weight of trimethylolpropane triglycidyl ether, 3-10 parts by weight of the functionalized carbon nano tube prepared in the second step and 10-20 parts by weight of benzyl alcohol, filling the materials into a reaction kettle, fully stirring the materials at the temperature of 25-45 ℃, and fully and uniformly dispersing the functionalized carbon nano tube in the matching reinforcing and toughening liquid through ultrahigh frequency oscillation to finally prepare the matching reinforcing and toughening liquid.
5. The preparation method of the high-strength anti-yellowing freeze-thaw resistant epoxy resin for sponge city construction according to claim 1, wherein in the step (5), the added amount of each component is as follows: 100 parts of epoxy resin main agent is added with 40-50 parts of curing agent and 8-20 parts of matching reinforcing toughening liquid.
6. The preparation method of the high-strength anti-yellowing freeze-thaw-resistant epoxy resin for sponge city construction according to claim 1, wherein the stirring temperature in the step (5) is: 25-45 ℃.
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