CN113583392B - Normal-temperature in-situ repair material for drainage pipeline and construction method thereof - Google Patents

Normal-temperature in-situ repair material for drainage pipeline and construction method thereof Download PDF

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CN113583392B
CN113583392B CN202110849528.6A CN202110849528A CN113583392B CN 113583392 B CN113583392 B CN 113583392B CN 202110849528 A CN202110849528 A CN 202110849528A CN 113583392 B CN113583392 B CN 113583392B
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stirring
parts
drainage pipeline
uniformly
situ
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CN113583392A (en
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李通
李佳川
李万朝
张�杰
俞发兰
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Shanghai Yufan Environmental Technology Co ltd
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Shanghai Yufan Environmental Technology Co ltd
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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
    • C08L63/10—Epoxy resins modified by unsaturated compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
    • C08F220/32—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals
    • C08F220/325—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals containing glycidyl radical, e.g. glycidyl (meth)acrylate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/10—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
    • C08F283/105—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule on to unsaturated polymers containing more than one epoxy radical per molecule
    • E—FIXED CONSTRUCTIONS
    • E03—WATER SUPPLY; SEWERAGE
    • E03F—SEWERS; CESSPOOLS
    • E03F3/00—Sewer pipe-line systems
    • E03F3/06—Methods of, or installations for, laying sewer pipes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/18—Applications used for pipes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/18—Spheres
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A20/00—Water conservation; Efficient water supply; Efficient water use
    • Y02A20/20—Controlling water pollution; Waste water treatment

Abstract

The invention discloses a normal-temperature in-situ repair material for a drainage pipeline and a construction method thereof, wherein the normal-temperature in-situ repair material comprises a material A and a material B, wherein the material A is obtained by uniformly mixing phenolic epoxy acrylate, bisphenol A epoxy diacrylate and 2-ethyl methacrylate, and the material B is obtained by uniformly mixing 4-vinylbenzaldehyde, a photoinitiator 1173, azodiisobutyronitrile, coumarin-porous microsphere compound, titanium porphyrin compound, dichloromethane and trifluoroacetic acid. During construction, the material A and the material B are directly stirred and mixed uniformly, and the material A and the material B are prepared and used immediately, are convenient to use, have higher mechanical property and corrosion resistance, and have good repairability to a drainage pipeline.

Description

Normal-temperature in-situ repair material for drainage pipeline and construction method thereof
Technical Field
The invention relates to the technical field of pipeline repair, in particular to a normal-temperature in-situ repair material for a drainage pipeline and a construction method thereof.
Background
The in-situ curing repair process is one of the processes which are widely applied in the current drainage pipeline repair construction, and the construction processes which are widely applied in China at present comprise a turnover heat curing method, a pull-in ultraviolet curing method and the like.
The overturning heat curing repair construction needs enough overturning construction space on site, the pipe section to be repaired at least needs an inspection well at one end, the periphery of the inspection well is provided with a field and a space for placing overturning equipment, a hot water heating system and the like, and enough water is needed to ensure that overturning construction is smoothly carried out during heating.
The ultraviolet curing repair construction needs that inspection wells at two ends of a pipe section are provided with operation spaces, a lining hose is placed at the position of one inspection well, a winch is fixed at the other inspection well to pull materials, the requirements on the site of a construction site are strict, and the space and the site for placing curing equipment are needed in the curing process.
When the two repair processes are used for repairing pipelines below a road, the limiting factors of places do not need to be considered. However, when pipelines are distributed in river channels or are difficult to reach by vehicles, enough auxiliary facilities are needed to be erected to finish repair construction. For these special construction pipelines, especially pipelines limited by construction sites and environment, normal temperature in situ curing repair process can be adopted.
Patent application CN110746552a discloses an in-situ curing repair resin, which consists of a material a and a material B, wherein the material a comprises a curable resin, a reaction diluent, a crosslinking agent, a filler and the like, and the material B is a curing agent, and the curable resin comprises an acrylic resin, a polycarbonate resin, a polylactic acid resin, polyethylene glycol and the like. The resin of the patent application is poor in mechanical property after being cured, corrosion resistance mainly depends on the addition of nano silver powder, and is high in cost and unsatisfactory in repairing effect on a drainage pipeline.
Disclosure of Invention
The invention aims to provide a normal-temperature in-situ repair material for a drainage pipeline and a construction method thereof, which are used for improving mechanical properties and corrosion resistance and have good repair property for the drainage pipeline.
In order to achieve the above purpose, the invention is realized by the following scheme:
the normal-temperature in-situ repair material for the drainage pipeline comprises a material A and a material B, wherein the material A is prepared by uniformly mixing 100 parts of phenolic epoxy acrylate, 80-100 parts of bisphenol A epoxy diacrylate and 30-40 parts of 2-ethyl methacrylate in parts by weight;
the preparation method of the material B comprises the following steps:
(1) Firstly, preparing porous microspheres by using glycidyl methacrylate and ethylene glycol dimethacrylate as raw materials;
(2) Then adding the porous microspheres, 3-aminophenol and ethyl acetoacetate into absolute ethyl alcohol, and stirring and reacting by taking zinc chloride as a catalyst to obtain coumarin-porous microsphere compound;
(3) Then tetra (p-carboxyphenyl) porphyrin and titanium tetrachloride are used as raw materials to react under the protection of nitrogen to obtain a titanium porphyrin complex;
(4) Finally, evenly mixing 0.2 to 0.3 part of 4-vinylbenzaldehyde, 1 to 2 parts of photoinitiator 1173, 1 to 2 parts of azodiisobutyronitrile, 1 to 2 parts of coumarin-porous microsphere compound, 0.3 to 0.5 part of titanium porphyrin compound, 7 to 9 parts of dichloromethane and 1 to 2 parts of trifluoroacetic acid.
Preferably, the specific method of the step (1) comprises the following steps of: firstly, uniformly stirring and mixing 50-60 parts of glycidyl methacrylate, 35-45 parts of ethylene glycol dimethacrylate, 35-45 parts of diethyl phthalate and 2-3 parts of benzoyl peroxide to obtain an oil phase; then adding 8-10 parts of polyvinyl alcohol into 1000 parts of water, and stirring and uniformly mixing to obtain a water phase; then slowly and uniformly dripping the oil phase into the water phase while stirring, stirring and reacting for 3-4 hours at 80-85 ℃ and 500-600 r/min after dripping, naturally cooling to room temperature, centrifuging, and washing with water to obtain the porous microspheres. Feeding in
Preferably, the one-step dripping time of the oil phase is 30-40 minutes, and the particle size of the porous microspheres is 5
And μm or less.
Preferably, the specific method of the step (2) is as follows in parts by weight: firstly adding 1 part of porous microsphere, 0.3-0.5 part of 3-aminophenol and 0.2-0.3 part of ethyl acetoacetate into 5-7 parts of absolute ethyl alcohol, stirring and uniformly mixing, then adding 0.3-0.5 part of zinc chloride, heating to reflux under the protection of nitrogen, preserving heat and stirring for reaction, naturally cooling to room temperature after the reaction is finished, adding 4-5 parts of hydrochloric acid with the mass concentration of 36-38%, stirring and uniformly mixing, filtering, washing with water and drying to obtain the coumarin-porous microsphere compound.
More preferably, the reaction time is 6 to 8 hours.
Preferably, the specific method of the step (3) is as follows: adding 1 part of tetra (p-carboxyphenyl) porphyrin into 4-5 parts of N, N' -dimethylformamide, stirring and dispersing uniformly, then adding 1-2 parts of pyridine, stirring and mixing uniformly, then adding 0.02-0.03 part of titanium tetrachloride under the protection of nitrogen while stirring, stirring and reacting, and performing post-treatment to obtain the titanium porphyrin complex.
Further preferably, the process conditions of the stirring reaction are: stirring and reacting for 5-6 hours at 140-150 ℃.
Further preferably, the specific method of post-treatment is as follows: the volume ratio is 6:1, performing silica gel column chromatography separation on the chloroform-methanol mixed solution, removing the solvent by rotary evaporation, and drying.
According to the construction method of the normal-temperature in-situ repair material for the drainage pipeline, the material A and the material B are uniformly stirred to obtain the resin mother solution, the hose is fully immersed by the resin mother solution and rolled to the designed thickness, then the hose is subjected to overturning construction by adopting the gas overturning equipment, the hose is pushed to the position to be repaired by using the air compressor, and the hose is continuously inflated into the hose to enable the hose to be closely attached to the pipeline to be repaired, the air pressure is maintained, the curing reaction is carried out, and the equipment is removed after the curing is completed.
Preferably, the dipping time is 10-15 minutes, the air pressure is maintained to be 0.5-0.8 MPa, and the curing reaction time is 20-30 minutes.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a normal-temperature in-situ repair material for a drainage pipeline, which comprises a material A and a material B, wherein the material A is prepared by uniformly mixing phenolic epoxy acrylate, bisphenol A epoxy diacrylate and 2-ethyl methacrylate, and the material B is prepared by uniformly mixing 4-vinylbenzaldehyde, a photoinitiator 1173, azodiisobutyronitrile, a coumarin-porous microsphere compound, a titanium porphyrin compound, methylene dichloride and trifluoroacetic acid. During construction, the material A and the material B are directly stirred and mixed uniformly, and the material A and the material B are prepared and used immediately, are convenient to use, have higher mechanical property and corrosion resistance, and have good repairability to a drainage pipeline. The advantages of the invention are as follows:
1. the whole repair construction can be completed only by the air compressor and the air overturning platform on the construction site, and additional water source supply and material pulling equipment are not needed, so that the method is particularly suitable for pipeline repair construction which is difficult to directly reach on the construction site.
2. The curing process does not require a boiler or a photo-curing vehicle, only requires maintaining the hose at a sufficient air pressure during the curing process, and only requires an air compressor to maintain the pressure during the curing process.
3. The hose is impregnated and pressed on site, so that the problem that the lining hose is solidified in the transportation process is avoided, and the construction time can be reasonably and timely arranged according to the dredging condition of the site. And the whole construction time is comprehensively coordinated.
4. The construction process has higher requirements for engineering personnel, the whole construction process is reasonably arranged according to the curing time of the resin, the resin is installed in place before curing, and the whole construction process can be intuitively displayed for the projects with urgent requirements.
5. The material B comprises two key components, namely a titanium porphyrin complex and a coumarin-porous microsphere complex. Wherein, the titanium porphyrin complex plays a role of a catalyst to promote resin polymerization, and the special space structure can promote polymerization branching of the epoxy structure to be more abundant, and the formation of the branching structure is favorable for improving mechanical property and corrosion resistance; the coumarin-porous microsphere compound plays a role of filler, is uniformly dispersed in the system, and further improves mechanical properties and corrosion resistance.
The coumarin-porous microsphere compound is prepared by firstly preparing porous microspheres from glycidyl methacrylate and ethylene glycol dimethacrylate, then adding the porous microspheres, 3-aminophenol and ethyl acetoacetate into absolute ethyl alcohol, and stirring and reacting with zinc chloride as a catalyst, wherein in the process, the generated coumarin is deposited on the surfaces or in pores of the porous microspheres, the particle size of the compound is controlled, the uniform dispersion of the compound in a system is ensured, and meanwhile, the porous microspheres play a role in buffering, so that the mechanical performance and corrosion resistance are improved.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The normal-temperature in-situ repair material for the drainage pipeline comprises a material A and a material B, wherein the material A is prepared by uniformly mixing 100kg of phenolic epoxy acrylate, 80kg of bisphenol A epoxy diacrylate and 40kg of 2-ethyl methacrylate;
the preparation method of the material B comprises the following steps:
(1) Firstly, preparing porous microspheres by using glycidyl methacrylate and ethylene glycol dimethacrylate as raw materials;
(2) Then adding the porous microspheres, 3-aminophenol and ethyl acetoacetate into absolute ethyl alcohol, and stirring and reacting by taking zinc chloride as a catalyst to obtain coumarin-porous microsphere compound;
(3) Then tetra (p-carboxyphenyl) porphyrin and titanium tetrachloride are used as raw materials to react under the protection of nitrogen to obtain a titanium porphyrin complex;
(4) Finally, evenly mixing 0.2kg of 4-vinylbenzaldehyde, 2kg of photoinitiator 1173, 1kg of azodiisobutyronitrile, 2kg of coumarin-porous microsphere compound, 0.3kg of titanium porphyrin complex, 9kg of dichloromethane and 1kg of trifluoroacetic acid.
The specific method of the step (1) comprises the following steps: firstly, 60kg of glycidyl methacrylate, 35kg of ethylene glycol dimethacrylate, 45kg of diethyl phthalate and 2kg of benzoyl peroxide are stirred and mixed uniformly to obtain an oil phase; then adding 10kg of polyvinyl alcohol into 1000kg of water, and stirring and uniformly mixing to obtain a water phase; then slowly and uniformly dripping the oil phase into the water phase while stirring, stirring and reacting for 3 hours at 80 ℃ and 600r/min after the dripping, naturally cooling to room temperature, centrifuging, and washing with water to obtain the porous microspheres.
The dripping time of the oil phase is 40 minutes, and the particle size of the porous microsphere is below 5 mu m.
The specific method of the step (2) is as follows: firstly adding 1kg of porous microspheres, 0.3kg of 3-aminophenol and 0.3kg of ethyl acetoacetate into 5kg of absolute ethyl alcohol, stirring and mixing uniformly, then adding 0.5kg of zinc chloride, heating to reflux under the protection of nitrogen, preserving heat and stirring for reaction, naturally cooling to room temperature after the reaction is finished, adding 4kg of hydrochloric acid with the mass concentration of 38%, stirring and mixing uniformly, filtering, washing with water and drying to obtain the coumarin-porous microsphere compound.
The reaction time was 6 hours.
The specific method of the step (3) is as follows: firstly adding 1kg of tetra (p-carboxyphenyl) porphyrin into 5kg of N, N' -dimethylformamide, stirring and dispersing uniformly, then adding 1kg of pyridine, stirring and mixing uniformly, then adding 0.03kg of titanium tetrachloride under the protection of nitrogen while stirring, stirring and reacting, and performing post-treatment to obtain the titanium porphyrin complex.
The technological conditions of the stirring reaction are as follows: the reaction was stirred at 140℃for 6 hours.
The specific method for post-treatment comprises the following steps: the volume ratio is 6:1, performing silica gel column chromatography separation on the chloroform-methanol mixed solution, removing the solvent by rotary evaporation, and drying.
Example 2
The normal-temperature in-situ repair material for the drainage pipeline comprises a material A and a material B, wherein the material A is prepared by uniformly mixing 100kg of phenolic epoxy acrylate, 100kg of bisphenol A epoxy diacrylate and 30kg of 2-ethyl methacrylate;
the preparation method of the material B comprises the following steps:
(1) Firstly, preparing porous microspheres by using glycidyl methacrylate and ethylene glycol dimethacrylate as raw materials;
(2) Then adding the porous microspheres, 3-aminophenol and ethyl acetoacetate into absolute ethyl alcohol, and stirring and reacting by taking zinc chloride as a catalyst to obtain coumarin-porous microsphere compound;
(3) Then tetra (p-carboxyphenyl) porphyrin and titanium tetrachloride are used as raw materials to react under the protection of nitrogen to obtain a titanium porphyrin complex;
(4) Finally, evenly mixing 0.3kg of 4-vinylbenzaldehyde, 1kg of photoinitiator 1173, 2kg of azodiisobutyronitrile, 1kg of coumarin-porous microsphere compound, 0.5kg of titanium porphyrin complex, 7kg of dichloromethane and 2kg of trifluoroacetic acid.
The specific method of the step (1) comprises the following steps: firstly, uniformly stirring and mixing 50kg of glycidyl methacrylate, 45kg of ethylene glycol dimethacrylate, 35kg of diethyl phthalate and 3kg of benzoyl peroxide to obtain an oil phase; then adding 8kg of polyvinyl alcohol into 1000kg of water, and stirring and uniformly mixing to obtain a water phase; then slowly and uniformly dripping the oil phase into the water phase while stirring, stirring and reacting for 4 hours at 85 ℃ and 500r/min after the dripping, naturally cooling to room temperature, centrifuging, and washing with water to obtain the porous microspheres.
The dripping time of the oil phase is 30 minutes, and the particle size of the porous microsphere is below 5 mu m.
The specific method of the step (2) is as follows: firstly adding 1kg of porous microspheres, 0.5kg of 3-aminophenol and 0.2kg of ethyl acetoacetate into 7kg of absolute ethyl alcohol, stirring and mixing uniformly, then adding 0.3kg of zinc chloride, heating to reflux under the protection of nitrogen, preserving heat and stirring for reaction, naturally cooling to room temperature after the reaction is finished, adding 5kg of hydrochloric acid with the mass concentration of 36%, stirring and mixing uniformly, filtering, washing with water and drying to obtain the coumarin-porous microsphere compound.
The reaction time was 8 hours.
The specific method of the step (3) is as follows: adding 1kg of tetra (p-carboxyphenyl) porphyrin into 4kg of N, N' -dimethylformamide, stirring and dispersing uniformly, then adding 2kg of pyridine, stirring and mixing uniformly, then adding 0.02kg of titanium tetrachloride under the protection of nitrogen while stirring, stirring and reacting, and performing post-treatment to obtain the titanium porphyrin complex.
The technological conditions of the stirring reaction are as follows: the reaction was stirred at 150℃for 5 hours.
The specific method for post-treatment comprises the following steps: the volume ratio is 6:1, performing silica gel column chromatography separation on the chloroform-methanol mixed solution, removing the solvent by rotary evaporation, and drying.
Example 3
A normal-temperature in-situ repair material for a drainage pipeline comprises a material A and a material B, wherein the material A is prepared by uniformly mixing 100kg of phenolic epoxy acrylate, 90kg of bisphenol A epoxy diacrylate and 35kg of 2-ethyl methacrylate;
the preparation method of the material B comprises the following steps:
(1) Firstly, preparing porous microspheres by using glycidyl methacrylate and ethylene glycol dimethacrylate as raw materials;
(2) Then adding the porous microspheres, 3-aminophenol and ethyl acetoacetate into absolute ethyl alcohol, and stirring and reacting by taking zinc chloride as a catalyst to obtain coumarin-porous microsphere compound;
(3) Then tetra (p-carboxyphenyl) porphyrin and titanium tetrachloride are used as raw materials to react under the protection of nitrogen to obtain a titanium porphyrin complex;
(4) Finally, evenly mixing 0.25kg of 4-vinylbenzaldehyde, 1.5kg of photoinitiator 1173, 1.5kg of azodiisobutyronitrile, 1.5kg of coumarin-porous microsphere compound, 0.4kg of titanium porphyrin complex, 8kg of dichloromethane and 1.5kg of trifluoroacetic acid.
The specific method of the step (1) comprises the following steps: firstly, uniformly stirring and mixing 55kg of glycidyl methacrylate, 40kg of ethylene glycol dimethacrylate, 40kg of diethyl phthalate and 2.5kg of benzoyl peroxide to obtain an oil phase; then adding 9kg of polyvinyl alcohol into 1000kg of water, and stirring and uniformly mixing to obtain a water phase; then slowly and uniformly dripping the oil phase into the water phase while stirring, stirring and reacting for 3.5 hours at 82 ℃ and 600r/min after the dripping, naturally cooling to room temperature, centrifuging, and washing with water to obtain the porous microspheres.
The drop time of the oil phase is 35 minutes, and the particle size of the porous microsphere is below 5 μm.
The specific method of the step (2) is as follows: adding 1kg of porous microspheres, 0.4kg of 3-aminophenol and 0.25kg of ethyl acetoacetate into 6kg of absolute ethyl alcohol, stirring and uniformly mixing, then adding 0.4kg of zinc chloride, heating to reflux under the protection of nitrogen, preserving heat and stirring for reaction, naturally cooling to room temperature after the reaction is finished, adding 4.5kg of hydrochloric acid with the mass concentration of 37%, stirring and uniformly mixing, filtering, washing with water and drying to obtain the coumarin-porous microsphere compound.
The reaction time was 7 hours.
The specific method of the step (3) is as follows: adding 1kg of tetra (p-carboxyphenyl) porphyrin into 4.5kg of N, N' -dimethylformamide, stirring and dispersing uniformly, adding 1.5kg of pyridine, stirring and mixing uniformly, adding 0.025kg of titanium tetrachloride under the protection of nitrogen, stirring and reacting, and performing post-treatment to obtain the titanium porphyrin complex.
The technological conditions of the stirring reaction are as follows: the reaction was stirred at 145℃for 5.5 hours.
The specific method for post-treatment comprises the following steps: the volume ratio is 6:1, performing silica gel column chromatography separation on the chloroform-methanol mixed solution, removing the solvent by rotary evaporation, and drying.
Comparative example 1
The normal-temperature in-situ repair material for the drainage pipeline comprises a material A and a material B, wherein the material A is prepared by uniformly mixing 100kg of phenolic epoxy acrylate, 80kg of bisphenol A epoxy diacrylate and 40kg of 2-ethyl methacrylate;
the preparation method of the material B comprises the following steps:
(1) Firstly, preparing porous microspheres by using glycidyl methacrylate and ethylene glycol dimethacrylate as raw materials;
(2) Then, tetra (p-carboxyphenyl) porphyrin and titanium tetrachloride are used as raw materials to react under the protection of nitrogen to obtain a titanium porphyrin complex;
(3) Finally, uniformly mixing 0.2kg of 4-vinyl benzaldehyde, 2kg of photoinitiator 1173, 1kg of azodiisobutyronitrile, 2kg of porous microspheres, 0.3kg of titanium porphyrin complex, 9kg of dichloromethane and 1kg of trifluoroacetic acid.
The specific method of the step (1) comprises the following steps: firstly, 60kg of glycidyl methacrylate, 35kg of ethylene glycol dimethacrylate, 45kg of diethyl phthalate and 2kg of benzoyl peroxide are stirred and mixed uniformly to obtain an oil phase; then adding 10kg of polyvinyl alcohol into 1000kg of water, and stirring and uniformly mixing to obtain a water phase; then slowly and uniformly dripping the oil phase into the water phase while stirring, stirring and reacting for 3 hours at 80 ℃ and 600r/min after the dripping, naturally cooling to room temperature, centrifuging, and washing with water to obtain the porous microspheres.
The dripping time of the oil phase is 40 minutes, and the particle size of the porous microsphere is below 5 mu m.
The specific method of the step (2) is as follows: firstly adding 1kg of tetra (p-carboxyphenyl) porphyrin into 5kg of N, N' -dimethylformamide, stirring and dispersing uniformly, then adding 1kg of pyridine, stirring and mixing uniformly, then adding 0.03kg of titanium tetrachloride under the protection of nitrogen while stirring, stirring and reacting, and performing post-treatment to obtain the titanium porphyrin complex.
The technological conditions of the stirring reaction are as follows: the reaction was stirred at 140℃for 6 hours.
The specific method for post-treatment comprises the following steps: the volume ratio is 6:1, performing silica gel column chromatography separation on the chloroform-methanol mixed solution, removing the solvent by rotary evaporation, and drying.
Comparative example 2
The normal-temperature in-situ repair material for the drainage pipeline comprises a material A and a material B, wherein the material A is prepared by uniformly mixing 100kg of phenolic epoxy acrylate, 80kg of bisphenol A epoxy diacrylate and 40kg of 2-ethyl methacrylate;
the preparation method of the material B comprises the following steps:
(1) Then tetra (p-carboxyphenyl) porphyrin and titanium tetrachloride are used as raw materials to react under the protection of nitrogen to obtain a titanium porphyrin complex;
(2) Finally, evenly mixing 0.2kg of 4-vinyl benzaldehyde, 2kg of photoinitiator 1173, 1kg of azodiisobutyronitrile, 0.3kg of titanium porphyrin complex, 9kg of dichloromethane and 1kg of trifluoroacetic acid.
The specific method of the step (1) is as follows: firstly adding 1kg of tetra (p-carboxyphenyl) porphyrin into 5kg of N, N' -dimethylformamide, stirring and dispersing uniformly, then adding 1kg of pyridine, stirring and mixing uniformly, then adding 0.03kg of titanium tetrachloride under the protection of nitrogen while stirring, stirring and reacting, and performing post-treatment to obtain the titanium porphyrin complex.
The technological conditions of the stirring reaction are as follows: the reaction was stirred at 140℃for 6 hours.
The specific method for post-treatment comprises the following steps: the volume ratio is 6:1, performing silica gel column chromatography separation on the chloroform-methanol mixed solution, removing the solvent by rotary evaporation, and drying.
Comparative example 3
The normal-temperature in-situ repair material for the drainage pipeline comprises a material A and a material B, wherein the material A is prepared by uniformly mixing 100kg of phenolic epoxy acrylate, 80kg of bisphenol A epoxy diacrylate and 40kg of 2-ethyl methacrylate;
the preparation method of the material B comprises the following steps:
(1) Firstly, preparing porous microspheres by using glycidyl methacrylate and ethylene glycol dimethacrylate as raw materials;
(2) Then adding the porous microspheres, 3-aminophenol and ethyl acetoacetate into absolute ethyl alcohol, and stirring and reacting by taking zinc chloride as a catalyst to obtain coumarin-porous microsphere compound;
(3) Finally, evenly mixing 0.2kg of 4-vinylbenzaldehyde, 2kg of photoinitiator 1173, 1kg of azodiisobutyronitrile, 2kg of coumarin-porous microsphere compound, 0.3kg of cobalt acetate, 9kg of dichloromethane and 1kg of trifluoroacetic acid.
The specific method of the step (1) comprises the following steps: firstly, 60kg of glycidyl methacrylate, 35kg of ethylene glycol dimethacrylate, 45kg of diethyl phthalate and 2kg of benzoyl peroxide are stirred and mixed uniformly to obtain an oil phase; then adding 10kg of polyvinyl alcohol into 1000kg of water, and stirring and uniformly mixing to obtain a water phase; then slowly and uniformly dripping the oil phase into the water phase while stirring, stirring and reacting for 3 hours at 80 ℃ and 600r/min after the dripping, naturally cooling to room temperature, centrifuging, and washing with water to obtain the porous microspheres.
The dripping time of the oil phase is 40 minutes, and the particle size of the porous microsphere is below 5 mu m.
The specific method of the step (2) is as follows: firstly adding 1kg of porous microspheres, 0.3kg of 3-aminophenol and 0.3kg of ethyl acetoacetate into 5kg of absolute ethyl alcohol, stirring and mixing uniformly, then adding 0.5kg of zinc chloride, heating to reflux under the protection of nitrogen, preserving heat and stirring for reaction, naturally cooling to room temperature after the reaction is finished, adding 4kg of hydrochloric acid with the mass concentration of 38%, stirring and mixing uniformly, filtering, washing with water and drying to obtain the coumarin-porous microsphere compound.
The reaction time was 6 hours.
The repair materials obtained in examples 1 to 3 and comparative examples 1 to 3 were used for repairing a drain pipe, respectively, and the specific method was as follows: the material A and the material B are stirred and mixed uniformly to obtain resin mother liquor, then the hose is fully impregnated with the resin mother liquor (the impregnation time is 12 minutes), rolled to the designed thickness, then the hose is overturned by adopting gas overturning equipment, the hose is pushed to a position to be repaired by utilizing an air compressor, the hose is continuously inflated into the hose to enable the hose to be tightly attached to a pipeline to be repaired, the air pressure is maintained to be 0.7Ma, the curing reaction (the curing reaction time is 25 minutes), and the equipment is removed after the curing is completed.
The mechanical properties and corrosion resistance were examined with reference to ASTM F1216, and the results are shown in tables 1 and 2.
When corrosion resistance was examined, a blank was set by contacting with corrosive substances at 23℃for one month, and mechanical properties were again measured after one month, and flexural strength of the blank was 148.7MPa.
TABLE 1 investigation of mechanical Properties
Figure BDA0003181896450000121
TABLE 2 investigation of corrosion resistance
Figure BDA0003181896450000122
Figure BDA0003181896450000131
As is clear from tables 1 and 2, the repairing materials obtained in examples 1 to 3 were used to repair drain pipes, and were excellent in mechanical properties and corrosion resistance. And is superior to the performance of comparative examples 1 to 3.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.

Claims (10)

1. The normal-temperature in-situ repair material for the drainage pipeline is characterized by comprising a material A and a material B, wherein the material A is prepared by uniformly mixing 100 parts of phenolic epoxy acrylate, 80-100 parts of bisphenol A epoxy diacrylate and 30-40 parts of 2-ethyl methacrylate in parts by weight;
the preparation method of the material B comprises the following steps:
(1) Firstly, preparing porous microspheres by using glycidyl methacrylate and ethylene glycol dimethacrylate as raw materials;
(2) Then adding the porous microspheres, 3-aminophenol and ethyl acetoacetate into absolute ethyl alcohol, and stirring and reacting by taking zinc chloride as a catalyst to obtain coumarin-porous microsphere compound;
(3) Then tetra (p-carboxyphenyl) porphyrin and titanium tetrachloride are used as raw materials to react under the protection of nitrogen to obtain a titanium porphyrin complex;
(4) Finally, evenly mixing 0.2 to 0.3 part of 4-vinylbenzaldehyde, 1 to 2 parts of photoinitiator 1173, 1 to 2 parts of azodiisobutyronitrile, 1 to 2 parts of coumarin-porous microsphere compound, 0.3 to 0.5 part of titanium porphyrin compound, 7 to 9 parts of dichloromethane and 1 to 2 parts of trifluoroacetic acid.
2. The normal temperature in situ repairing material for a drainage pipeline according to claim 1, wherein the specific method of the step (1) is as follows in parts by weight: firstly, uniformly stirring and mixing 50-60 parts of glycidyl methacrylate, 35-45 parts of ethylene glycol dimethacrylate, 35-45 parts of diethyl phthalate and 2-3 parts of benzoyl peroxide to obtain an oil phase; then adding 8-10 parts of polyvinyl alcohol into 1000 parts of water, and stirring and uniformly mixing to obtain a water phase; then slowly and uniformly dripping the oil phase into the water phase while stirring, stirring and reacting for 3-4 hours at 80-85 ℃ and 500-600 r/min after dripping, naturally cooling to room temperature, centrifuging, and washing with water to obtain the porous microspheres.
3. The normal temperature in situ repairing material for drainage pipeline according to claim 1, wherein the dripping time of the oil phase is 30-40 minutes, and the particle size of the porous microspheres is below 5 μm.
4. The normal temperature in-situ repairing material for a drainage pipeline according to claim 1, wherein the specific method of the step (2) is as follows in parts by weight: firstly adding 1 part of porous microsphere, 0.3-0.5 part of 3-aminophenol and 0.2-0.3 part of ethyl acetoacetate into 5-7 parts of absolute ethyl alcohol, stirring and uniformly mixing, then adding 0.3-0.5 part of zinc chloride, heating to reflux under the protection of nitrogen, preserving heat and stirring for reaction, naturally cooling to room temperature after the reaction is finished, adding 4-5 parts of hydrochloric acid with the mass concentration of 36-38%, stirring and uniformly mixing, filtering, washing with water and drying to obtain the coumarin-porous microsphere compound.
5. The normal temperature in situ repairing material for drainage pipeline according to claim 4, wherein the reaction time is 6-8 hours.
6. The normal temperature in-situ repairing material for a drainage pipeline according to claim 1, wherein the specific method of the step (3) is as follows in parts by weight: adding 1 part of tetra (p-carboxyphenyl) porphyrin into 4-5 parts of N, N' -dimethylformamide, stirring and dispersing uniformly, then adding 1-2 parts of pyridine, stirring and mixing uniformly, then adding 0.02-0.03 part of titanium tetrachloride under the protection of nitrogen while stirring, stirring and reacting, and performing post-treatment to obtain the titanium porphyrin complex.
7. The normal temperature in situ repair material for a drain pipeline according to claim 6, wherein the process conditions of the stirring reaction are as follows: stirring and reacting for 5-6 hours at 140-150 ℃.
8. The normal temperature in situ restoration material for a drainage pipeline according to claim 6, wherein the specific method of post-treatment is as follows: the volume ratio is 6:1, performing silica gel column chromatography separation on the chloroform-methanol mixed solution, removing the solvent by rotary evaporation, and drying.
9. A construction method of a normal temperature in-situ repair material for a drainage pipeline according to any one of claims 1 to 8 is characterized in that firstly, materials A and B are stirred and mixed uniformly to obtain resin mother liquor, then a hose is fully immersed by the resin mother liquor and rolled to a designed thickness, then a gas turnover device is adopted to perform turnover construction on the hose, the hose is pushed to a position to be repaired by an air compressor, the hose is continuously inflated to enable the hose to be tightly attached to the pipeline to be repaired, air pressure is maintained, a curing reaction occurs, and the device is removed after the curing is completed.
10. The construction method for normal temperature in situ repairing material for drainage pipeline according to claim 9, wherein an immersion time is 10-15 minutes, a gas pressure is maintained at 0.5-0.8 MPa, and a curing reaction time is 20-30 minutes.
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