CN113480235A - High-strength epoxy resin repair mortar and preparation method thereof - Google Patents
High-strength epoxy resin repair mortar and preparation method thereof Download PDFInfo
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- CN113480235A CN113480235A CN202110897420.4A CN202110897420A CN113480235A CN 113480235 A CN113480235 A CN 113480235A CN 202110897420 A CN202110897420 A CN 202110897420A CN 113480235 A CN113480235 A CN 113480235A
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 100
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 100
- 239000004570 mortar (masonry) Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- 230000008439 repair process Effects 0.000 title claims abstract description 34
- 239000002904 solvent Substances 0.000 claims abstract description 64
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 55
- 239000010703 silicon Substances 0.000 claims abstract description 55
- 229920001577 copolymer Polymers 0.000 claims abstract description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- 239000003365 glass fiber Substances 0.000 claims abstract description 23
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 22
- 239000000178 monomer Substances 0.000 claims abstract description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000006004 Quartz sand Substances 0.000 claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims description 123
- 238000010438 heat treatment Methods 0.000 claims description 63
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 57
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 34
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 34
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 26
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 20
- 238000010276 construction Methods 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 20
- 239000008096 xylene Substances 0.000 claims description 20
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000011698 potassium fluoride Substances 0.000 claims description 13
- 235000003270 potassium fluoride Nutrition 0.000 claims description 13
- 238000011084 recovery Methods 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000004821 distillation Methods 0.000 claims description 12
- SZIFAVKTNFCBPC-UHFFFAOYSA-N 2-chloroethanol Chemical compound OCCCl SZIFAVKTNFCBPC-UHFFFAOYSA-N 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 7
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 6
- QYBKVVRRGQSGDC-UHFFFAOYSA-N triethyl methyl silicate Chemical compound CCO[Si](OC)(OCC)OCC QYBKVVRRGQSGDC-UHFFFAOYSA-N 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 5
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000010292 electrical insulation Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 18
- 230000000844 anti-bacterial effect Effects 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000006378 damage Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- GGDYAKVUZMZKRV-UHFFFAOYSA-N 2-fluoroethanol Chemical compound OCCF GGDYAKVUZMZKRV-UHFFFAOYSA-N 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 230000000711 cancerogenic effect Effects 0.000 description 2
- 231100000357 carcinogen Toxicity 0.000 description 2
- 239000003183 carcinogenic agent Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- -1 fluoroethyl p-toluenesulfonate Chemical compound 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- XNRDLSNSMTUXBV-UHFFFAOYSA-N 2-fluoroethyl 4-methylbenzenesulfonate Chemical compound CC1=CC=C(S(=O)(=O)OCCF)C=C1 XNRDLSNSMTUXBV-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- XENVCRGQTABGKY-ZHACJKMWSA-N chlorohydrin Chemical compound CC#CC#CC#CC#C\C=C\C(Cl)CO XENVCRGQTABGKY-ZHACJKMWSA-N 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/14—Polyepoxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/72—Repairing or restoring existing buildings or building materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses high-strength epoxy resin repair mortar and a preparation method thereof, wherein the repair mortar comprises a component A and a curing agent, the component A and the curing agent are mixed according to the mass ratio of 3-5:1, the component A is prepared from the following raw materials, by weight, 50-60 parts of modified epoxy resin, 40-50 parts of quartz sand and 10-15 parts of glass fiber, the modified epoxy resin is prepared from epoxy resin, p-toluenesulfonic acid, an organic silicon copolymer and a solvent, and the organic silicon copolymer is prepared from an organic silicon monomer, ethyl orthosilicate, ethanol and sodium carbonate. The main reason why the epoxy resin is used as the repair mortar in the invention is that the epoxy resin has certain chemical resistance, heat resistance and electrical insulation performance, and the mortar prepared by using the epoxy resin as the raw material has stronger adhesive force effect.
Description
Technical Field
The invention relates to the technical field of repair mortar preparation, in particular to high-strength epoxy resin repair mortar and a preparation method thereof.
Background
The epoxy resin is a high molecular polymer, and is a thermosetting resin commonly used in the market at present, because the epoxy resin contains a large amount of epoxy groups on the structure, after active hydrogen is added, the epoxy resin can be subjected to ring opening and further curing and crosslinking in the presence of the active hydrogen; the epoxy resin has excellent chemical resistance, heat resistance and insulativity, and the formed paint film has strong adhesive force and strong color retention property, thereby having wide application in the field of repair mortar.
The organosilicon copolymer is a polymer which contains silicon element in the molecular structure and is connected with organic functional groups on silicon atoms. The modified epoxy resin has certain corrosion resistance and heat resistance, and the strength, chemical resistance and corrosion resistance of the epoxy resin can be improved by modifying the epoxy resin with the organic silicon copolymer.
However, a large amount of solvent is needed in the preparation process, and the solvent is removed by distillation and other methods after the preparation is finished, so that the qualified rate of the product is ensured, but the volatilization of the solvent can cause environmental pollution, and xylene contained in the solvent is a common carcinogen and can affect human health, so that the invention of the high-strength epoxy resin repair mortar and the preparation method thereof is particularly important.
Disclosure of Invention
The invention aims to provide high-strength epoxy resin repair mortar and a preparation method thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: the high-strength epoxy resin repair mortar comprises a component A and a curing agent, wherein the component A and the curing agent are mixed according to the mass ratio of 3-5: 1;
the component A is prepared from the following raw materials, by weight, 50-60 parts of modified epoxy resin, 40-50 parts of quartz sand and 10-15 parts of glass fiber.
Further, the modified epoxy resin is prepared from epoxy resin, p-toluenesulfonic acid, organic silicon copolymer and solvent.
Further, the organic silicon copolymer is prepared from organic silicon monomers, ethyl orthosilicate, ethanol and sodium carbonate.
Furthermore, the organic silicon monomer is one or a mixture of two of monomethyloxytriethoxysilane and dimethyldiethoxysilane.
Further, the solvent is a mixture of ethylene glycol, xylene and acetone;
the mass ratio of the ethylene glycol to the xylene to the acetone is 7:3: 1.
A preparation method of high-strength epoxy resin repair mortar comprises the following steps,
s1, preparation of organic silicon copolymer:
adding ethanol into ethyl orthosilicate, stirring for dissolving, adding deionized water and acid liquor, adjusting pH, heating and stirring, adding an organic silicon monomer, stirring uniformly, adding acid for adjusting pH, heating, adding sodium carbonate, and stirring uniformly to obtain an organic silicon copolymer;
s2, preparation of modified epoxy resin:
heating epoxy resin, adding the obtained organic silicon copolymer and solvent, stirring, adding p-toluenesulfonic acid after uniformly stirring, heating and stirring, carrying out reduced pressure distillation after the reaction is finished, and recovering the solvent to obtain modified epoxy resin;
s3, solvent recovery treatment:
cooling the recovered solvent, adding potassium fluoride, stirring and heating, adding chloroethanol, stirring, uniformly stirring, cooling, adding pyridine, and stirring to obtain a product A;
s4, preparation of the component A:
adding quartz sand, glass fiber and the product A into the obtained modified epoxy resin, stirring, and uniformly stirring to obtain a component A;
s5, construction:
during construction, the component A and the curing agent are mixed and stirred uniformly to obtain mortar, the obtained mortar is coated on the surface of the carrier to be treated, and the heating and curing are carried out to obtain the product.
According to the application, tetraethoxysilane and organic silicon monomers are used for preparing the organic copolymer, and the prepared organic silicon copolymer is used for modifying epoxy resin, so that modified epoxy resin is obtained. The tetraethoxysilane added in the application participates in the preparation of the organic silicon polymer, and on the other hand, the tetraethoxysilane can improve the adhesion degree of the quality inspection of the epoxy resin, the quartz sand and the glass fiber and can also improve the heat resistance of the product.
According to the application, the epoxy resin is modified, the prepared organic silicon copolymer is added for modification, the epoxy resin contains secondary hydroxyl, and alkoxy contained in the organic silicon copolymer can perform polycondensation reaction with the secondary hydroxyl, so that the modified epoxy resin is obtained. The p-toluenesulfonic acid added in the preparation process is used as a catalyst, and is distilled out along with the solvent through reduced pressure distillation after the preparation is finished.
Further, the concrete steps are as follows,
s1, preparation of organic silicon copolymer:
adding ethanol into tetraethoxysilane, stirring for dissolving, adding deionized water and hydrochloric acid, adjusting the pH value to 3-3.2, heating and stirring at the temperature of 29-32 ℃ for 1-1.3h, heating to 50-53 ℃ for 2-2.5h, adding an organic silicon monomer, stirring uniformly, adding acid for adjusting the pH value to 3-3.2, heating at the temperature of 68-72 ℃ for 4-4.2h, adding sodium carbonate, adjusting the pH value of the system to be alkaline, stirring uniformly, filtering, and removing ethanol to obtain an organic silicon copolymer;
s2, preparation of modified epoxy resin:
heating epoxy resin, adding the obtained organic silicon copolymer and a solvent, stirring, adding p-toluenesulfonic acid after uniformly stirring, heating and stirring at the temperature of 80-83 ℃, reacting for 3-3.2 hours, carrying out reduced pressure distillation after the reaction is finished, and recovering the solvent to obtain modified epoxy resin;
s3, solvent recovery treatment:
cooling the recovered solvent, adding potassium fluoride, stirring and heating, adding chloroethanol, stirring, uniformly stirring, cooling, adding pyridine, and stirring to obtain a product A;
s4, preparation of the component A:
adding quartz sand, glass fiber and the product A into the obtained modified epoxy resin, stirring, and uniformly stirring to obtain a component A;
s5, construction:
during construction, the component A and the curing agent are mixed and stirred uniformly to obtain mortar, the obtained mortar is coated on the surface of the carrier to be treated, and the heating and curing are carried out to obtain the product.
Further, the solvent recovery process of step S3, the steps are as follows,
cooling the recovered solvent at 25-30 ℃, adding potassium fluoride, stirring and heating at 170-180 ℃, adding chloroethanol, stirring for 3-4h, uniformly stirring, cooling at 0-3 ℃, adding pyridine, stirring for 3-3.5h, and adding the obtained product into the component A.
Further, the solvent recovery processing operation needs to be performed under a nitrogen atmosphere.
Compared with the prior art, the invention has the following beneficial effects: the epoxy resin is used as the main raw material of the repair mortar, because the epoxy resin has certain chemical resistance, heat resistance and electric insulation performance, and the mortar prepared by using the epoxy resin as the raw material has strong adhesive force and is widely applied to the aspect of repairing the mortar.
The solvent that this application will be retrieved retrieves the preparation, mainly contains ethylene glycol, xylene and acetone in the solvent of retrieving, and wherein still contain p-toluene sulfonic acid, potassium fluoride and chlorohydrin have been added to this application to 0-3 ℃ reacts, adds pyridine after the reaction finishes, can react with p-toluene sulfonic acid after adding pyridine, and then gets rid of p-toluene sulfonic acid, reduces the harm that produces the environment. After the reaction is finished, a new product of fluoroethyl p-toluenesulfonate is generated, and the fluoroethyl p-toluenesulfonate is an effective antibacterial agent and can act with pyridine simultaneously, so that the antibacterial performance of the product is improved.
The main substances in the solvent used in the method are ethylene glycol and xylene, the xylene is a carcinogen, and residual xylene can volatilize in the preparation process and the use process, so that the solvent is removed by reduced pressure distillation after the preparation, and the harm of the product to human bodies is reduced. According to the application, acetone is added to the lowest amount of xylene and the amount of ethylene glycol is increased, so that the toxicity of the acetone and the ethylene glycol is relatively low, and the environmental and human safety is further ensured.
The application adds the potassium fluoride in the recovery processing, the potassium fluoride that adds can react with ethylene glycol under microthermal environment, generate 2-fluoroethanol, the 2-fluoroethanol that obtains can regard as the antibacterial agent to use on the one hand, can improve the antibacterial property of product, and still participate in the reaction of getting rid of p-toluenesulfonic acid, and then obtain p-toluenesulfonic acid fluoroethyl ester, improve the antibacterial property of product, but because the chloroethanol that adds and the 2-fluoroethanol that produces have certain toxicity, have certain injury to the human body, consequently need control its addition when adding the product that obtains to first component, and then guarantee the antibacterial property of product, it is minimum to reduce the harm that the organic matter volatilizees in the use of product and produce the human body.
This application uses the organosilicon monomer to modify epoxy, and the organosilicon monomer has certain mechanical strength, uses the organosilicon monomer to modify the mechanical strength that can increase the product to epoxy. The glass fiber is added on the basis of the epoxy resin, the added glass fiber has certain mechanical strength, heat resistance and corrosion resistance, and the addition of the glass fiber can increase the mechanical strength and the corrosion resistance of a product.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The high-strength epoxy resin repair mortar comprises a component A and a curing agent, wherein the component A and the curing agent are mixed according to the mass ratio of 3: 1;
the component A is prepared from the following raw materials, by weight, 50 parts of modified epoxy resin, 40 parts of quartz sand and 10 parts of glass fiber;
the organic silicon monomer is methyl-oxy-triethoxy silane.
The solvent is a mixture of ethylene glycol, xylene and acetone;
the mass ratio of the ethylene glycol to the xylene to the acetone is 7:3: 1.
A preparation method of high-strength epoxy resin repair mortar comprises the following steps,
s1, preparation of organic silicon copolymer:
adding ethanol into tetraethoxysilane, stirring for dissolving, adding deionized water and hydrochloric acid, adjusting the pH value to 3, heating and stirring at the temperature of 29 ℃ for 1h, heating to 50 ℃ for 2h, adding an organic silicon monomer, stirring uniformly, adding acid for adjusting the pH value to 3, heating at the temperature of 68 ℃ for 4h, adding sodium carbonate, adjusting the pH value of the system to be alkaline, stirring uniformly, filtering, and removing the ethanol to obtain an organic silicon copolymer;
s2, preparation of modified epoxy resin:
heating epoxy resin, adding the obtained organic silicon copolymer and a solvent, stirring, adding p-toluenesulfonic acid after uniformly stirring, heating and stirring at the temperature of 80 ℃, reacting for 3 hours, carrying out reduced pressure distillation after the reaction is finished, and recovering the solvent to obtain modified epoxy resin;
s3, solvent recovery treatment:
cooling the recovered solvent at 25 ℃, introducing nitrogen, adding potassium fluoride, stirring and heating at 170 ℃, adding chloroethanol, stirring for 3 hours, uniformly stirring, cooling, adding pyridine, and stirring for 3 hours to obtain a product A;
s4, preparation of the component A:
adding quartz sand, glass fiber and the product A into the obtained modified epoxy resin, stirring, and uniformly stirring to obtain a component A;
s5, construction:
during construction, the component A and the curing agent are mixed and stirred uniformly to obtain mortar, the obtained mortar is coated on the surface of the carrier to be treated, and the heating and curing are carried out to obtain the product.
Example 2
The high-strength epoxy resin repair mortar comprises a component A and a curing agent, wherein the component A and the curing agent are mixed according to the mass ratio of 4: 1;
the component A is prepared from the following raw materials in parts by weight, 55 parts of modified epoxy resin, 45 parts of quartz sand and 13 parts of glass fiber;
the organic silicon monomer is a mixture of monomethyloxytriethoxysilane and dimethyldiethoxysilane.
The solvent is a mixture of ethylene glycol, xylene and acetone;
the mass ratio of the ethylene glycol to the xylene to the acetone is 7:3: 1.
A preparation method of high-strength epoxy resin repair mortar comprises the following steps,
s1, preparation of organic silicon copolymer:
adding ethanol into tetraethoxysilane, stirring for dissolving, adding deionized water and hydrochloric acid, adjusting the pH value to 3.1, heating and stirring at the temperature of 30 ℃ for 1.2h, heating to 52 ℃ for 2.3h, adding an organic silicon monomer, stirring uniformly, adding acid for adjusting the pH value to 3.1, heating at the temperature of 70 ℃ for 4.1h, adding sodium carbonate, adjusting the pH value of the system to be alkaline, filtering after stirring uniformly, and removing the ethanol to obtain an organic silicon copolymer;
s2, preparation of modified epoxy resin:
heating epoxy resin, adding the obtained organic silicon copolymer and a solvent, stirring, adding p-toluenesulfonic acid after uniformly stirring, heating and stirring at 82 ℃, reacting for 3.1h, carrying out reduced pressure distillation after the reaction is finished, and recovering the solvent to obtain modified epoxy resin;
s3, solvent recovery treatment:
cooling the recovered solvent, introducing nitrogen at the temperature of 27 ℃, adding potassium fluoride, stirring and heating, adding chloroethanol at the temperature of 175 ℃, stirring for 3.5 hours, uniformly stirring, cooling, adding pyridine at the temperature of 2 ℃, stirring for 3.2 hours to obtain a product A;
s4, preparation of the component A:
adding quartz sand, glass fiber and the product A into the obtained modified epoxy resin, stirring, and uniformly stirring to obtain a component A;
s5, construction:
during construction, the component A and the curing agent are mixed and stirred uniformly to obtain mortar, the obtained mortar is coated on the surface of the carrier to be treated, and the heating and curing are carried out to obtain the product.
Example 3
The high-strength epoxy resin repair mortar comprises a component A and a curing agent, wherein the component A and the curing agent are mixed according to the mass ratio of 5: 1;
the component A is prepared from the following raw materials in parts by weight, 60 parts of modified epoxy resin, 50 parts of quartz sand and 15 parts of glass fiber;
the organic silicon monomer is dimethyl diethoxy silane.
The solvent is a mixture of ethylene glycol, xylene and acetone;
the mass ratio of the ethylene glycol to the xylene to the acetone is 7:3: 1.
A preparation method of high-strength epoxy resin repair mortar comprises the following steps,
s1, preparation of organic silicon copolymer:
adding ethanol into tetraethoxysilane, stirring for dissolving, adding deionized water and hydrochloric acid, adjusting the pH value to 3.2, heating and stirring at the temperature of 32 ℃ for 1.3h, heating to 53 ℃, reacting for 2.5h, adding an organic silicon monomer, stirring uniformly, adding acid for adjusting the pH value to 3.2, heating at the temperature of 72 ℃ for 4.2h, adding sodium carbonate, adjusting the pH value of the system to be alkaline, filtering after stirring uniformly, and removing the ethanol to obtain an organic silicon copolymer;
s2, preparation of modified epoxy resin:
heating epoxy resin, adding the obtained organic silicon copolymer and a solvent, stirring, adding p-toluenesulfonic acid after uniformly stirring, heating and stirring at 83 ℃, reacting for 3.2 hours, carrying out reduced pressure distillation after the reaction is finished, and recovering the solvent to obtain modified epoxy resin;
s3, solvent recovery treatment:
cooling the recovered solvent at 30 ℃, introducing nitrogen, adding potassium fluoride, stirring and heating at 180 ℃, adding chloroethanol, stirring for 4 hours, uniformly stirring, cooling, adding pyridine, and stirring for 3.5 hours to obtain a product A;
s4, preparation of the component A:
adding quartz sand, glass fiber and the product A into the obtained modified epoxy resin, stirring, and uniformly stirring to obtain a component A;
s5, construction:
during construction, the component A and the curing agent are mixed and stirred uniformly to obtain mortar, the obtained mortar is coated on the surface of the carrier to be treated, and the heating and curing are carried out to obtain the product.
Comparative example 1
The high-strength epoxy resin repair mortar comprises a component A and a curing agent, wherein the component A and the curing agent are mixed according to the mass ratio of 5: 1;
the component A is prepared from the following raw materials in parts by weight, 60 parts of epoxy resin, 50 parts of quartz sand and 15 parts of glass fiber;
a preparation method of high-strength epoxy resin repair mortar comprises the following steps,
s1, preparation of the component A:
adding quartz sand, glass fiber and the product A into epoxy resin, stirring, and uniformly stirring to obtain a component A;
s2, construction:
during construction, the component A and the curing agent are mixed and stirred uniformly to obtain mortar, the obtained mortar is coated on the surface of the carrier to be treated, and the heating and curing are carried out to obtain the product.
Comparative example 2
The high-strength epoxy resin repair mortar comprises a component A and a curing agent, wherein the component A and the curing agent are mixed according to the mass ratio of 5: 1;
the component A is prepared from the following raw materials in parts by weight, 60 parts of modified epoxy resin, 50 parts of quartz sand and 15 parts of glass fiber;
the organic silicon monomer is dimethyl diethoxy silane.
The solvent is a mixture of ethylene glycol, xylene and acetone;
the mass ratio of the ethylene glycol to the xylene to the acetone is 7:3: 1.
A preparation method of high-strength epoxy resin repair mortar comprises the following steps,
s1, preparation of organic silicon copolymer:
adding ethanol into tetraethoxysilane, stirring for dissolving, adding deionized water and hydrochloric acid, adjusting the pH value to 3.2, heating and stirring at the temperature of 32 ℃ for 1.3h, heating to 53 ℃, reacting for 2.5h, adding an organic silicon monomer, stirring uniformly, adding acid for adjusting the pH value to 3.2, heating at the temperature of 72 ℃ for 4.2h, adding sodium carbonate, adjusting the pH value of the system to be alkaline, filtering after stirring uniformly, and removing the ethanol to obtain an organic silicon copolymer;
s2, preparation of modified epoxy resin:
heating epoxy resin, adding the obtained organic silicon copolymer and a solvent, stirring, adding p-toluenesulfonic acid after uniformly stirring, heating and stirring at 83 ℃, reacting for 3.2 hours, carrying out reduced pressure distillation after the reaction is finished, and recovering the solvent to obtain modified epoxy resin;
s3, preparation of the component A:
adding quartz sand and glass fiber into the obtained modified epoxy resin, stirring, and uniformly stirring to obtain a component A;
s5, construction:
during construction, the component A and the curing agent are mixed and stirred uniformly to obtain mortar, the obtained mortar is coated on the surface of the carrier to be treated, and the heating and curing are carried out to obtain the product.
Comparative example 3
The high-strength epoxy resin repair mortar comprises a component A and a curing agent, wherein the component A and the curing agent are mixed according to the mass ratio of 5: 1;
the component A is prepared from the following raw materials in parts by weight, 60 parts of modified epoxy resin, 50 parts of quartz sand and 15 parts of glass fiber;
the organic silicon monomer is dimethyl diethoxy silane.
The solvent is a mixture of ethylene glycol, xylene and acetone;
the mass ratio of the ethylene glycol to the xylene to the acetone is 7:3: 1.
A preparation method of high-strength epoxy resin repair mortar comprises the following steps,
s1, preparation of organic silicon copolymer:
adding ethanol into tetraethoxysilane, stirring for dissolving, adding deionized water and hydrochloric acid, adjusting the pH value to 3.2, heating and stirring at the temperature of 32 ℃ for 1.3h, heating to 53 ℃, reacting for 2.5h, adding an organic silicon monomer, stirring uniformly, adding acid for adjusting the pH value to 3.2, heating at the temperature of 72 ℃ for 4.2h, adding sodium carbonate, adjusting the pH value of the system to be alkaline, filtering after stirring uniformly, and removing the ethanol to obtain an organic silicon copolymer;
s2, preparation of modified epoxy resin:
heating epoxy resin, adding the obtained organic silicon copolymer and a solvent, stirring, adding p-toluenesulfonic acid after uniformly stirring, heating and stirring at 83 ℃, reacting for 3.2 hours, carrying out reduced pressure distillation after the reaction is finished, and recovering the solvent to obtain modified epoxy resin;
s3, solvent recovery treatment:
cooling the recovered solvent at 30 ℃, introducing nitrogen, adding potassium fluoride, stirring and heating at 180 ℃, adding chloroethanol, stirring for 4 hours, uniformly stirring, cooling, adding pyridine, and stirring for 3.5 hours to obtain a product A;
s4, preparation of the component A:
adding quartz sand, glass fiber and the product A into the obtained modified epoxy resin, stirring, and uniformly stirring to obtain a component A;
s5, construction:
during construction, the component A and the curing agent are mixed and stirred uniformly to obtain mortar, the obtained mortar is coated on the surface of the carrier to be treated, and the heating and curing are carried out to obtain the product.
Experiment of
And taking the example 3 as a control, and arranging a comparative example 1, a comparative example 2 and a comparative example 3, wherein the epoxy resin is not modified in the comparative example 1, the solvent is not recycled in the comparative example 2, and pyridine is not added in the solvent treatment in the comparative example 3 to carry out a control experiment.
Tensile strength and antibacterial property tests were performed on example 1, example 2, example 3, comparative example 1, comparative example 2, and comparative example 3, and the results were as follows,
watch 1
The epoxy resin is not modified in the comparative example 1, so that the tensile strength and the antibacterial rate of the comparative example 1 are lower than those of the examples 1, 2 and 3, which shows that the tensile strength of the product can be increased by modifying the epoxy resin with the organosilicon copolymer in the examples 1, 2 and 3, and the antibacterial rate of the product can be increased by adding the product after the solvent is recovered and the comprehensive performance of the product can be improved by adding the product in the examples 1, 2 and 3.
The fact that the solvent is not recovered in comparative example 2 results in the antibacterial ratio of comparative example 2 being lower than that of examples 1, 2 and 3 shows that the treated products of examples 1, 2 and 3, in which the solvent is added, have certain effects on the improvement of the antibacterial performance of the products.
In comparative example 3, no pyridine was added during the solvent treatment, which results in a lower antibacterial ratio in comparative example 3 compared to examples 1, 2 and 3, and it is demonstrated that pyridine can react with p-toluenesulfonic acid to obtain a product having antibacterial properties and further improve the comprehensive performance of the product after the pyridine is added in examples 1, 2 and 3.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. 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 (7)
1. A preparation method of high-strength epoxy resin repair mortar is characterized by comprising the following steps: the steps are as follows,
s1, preparation of organic silicon copolymer:
adding ethanol into ethyl orthosilicate, stirring for dissolving, adding deionized water and acid liquor, adjusting pH, heating and stirring, adding an organic silicon monomer, stirring uniformly, adding acid for adjusting pH, heating, adding sodium carbonate, and stirring uniformly to obtain an organic silicon copolymer;
s2, preparation of modified epoxy resin:
heating epoxy resin, adding the obtained organic silicon copolymer and solvent, stirring, adding p-toluenesulfonic acid after uniformly stirring, heating and stirring, carrying out reduced pressure distillation after the reaction is finished, and recovering the solvent to obtain modified epoxy resin;
s3, solvent recovery treatment:
cooling the recovered solvent, adding potassium fluoride, stirring and heating, adding chloroethanol, stirring, uniformly stirring, cooling, adding pyridine, and stirring to obtain a product A;
s4, preparation of the component A:
adding quartz sand, glass fiber and the product A into the obtained modified epoxy resin, stirring, and uniformly stirring to obtain a component A;
s5, construction:
during construction, the component A and the curing agent are mixed and stirred uniformly to obtain mortar, the obtained mortar is coated on the surface of the carrier to be treated, and the heating and curing are carried out to obtain the product.
2. The method for preparing the high-strength epoxy resin repair mortar according to claim 1, wherein the method comprises the following steps: the specific steps are as follows,
s1, preparation of organic silicon copolymer:
adding ethanol into tetraethoxysilane, stirring for dissolving, adding deionized water and hydrochloric acid, adjusting the pH value to 3-3.2, heating and stirring at the temperature of 29-32 ℃ for 1-1.3h, heating to 50-53 ℃ for 2-2.5h, adding an organic silicon monomer, stirring uniformly, adding acid for adjusting the pH value to 3-3.2, heating at the temperature of 68-72 ℃ for 4-4.2h, adding sodium carbonate, adjusting the pH value of the system to be alkaline, stirring uniformly, filtering, and removing ethanol to obtain an organic silicon copolymer;
s2, preparation of modified epoxy resin:
heating epoxy resin, adding the obtained organic silicon copolymer and a solvent, stirring, adding p-toluenesulfonic acid after uniformly stirring, heating and stirring at the temperature of 80-83 ℃, reacting for 3-3.2 hours, carrying out reduced pressure distillation after the reaction is finished, and recovering the solvent to obtain modified epoxy resin;
s3, solvent recovery treatment:
cooling the recovered solvent, adding potassium fluoride, stirring and heating, adding chloroethanol, stirring, uniformly stirring, cooling, adding pyridine, and stirring to obtain a product A;
s4, preparation of the component A:
adding quartz sand, glass fiber and the product A into the obtained modified epoxy resin, stirring, and uniformly stirring to obtain a component A;
s5, construction:
during construction, the component A and the curing agent are mixed and stirred uniformly to obtain mortar, the obtained mortar is coated on the surface of the carrier to be treated, and the heating and curing are carried out to obtain the product.
3. The method for preparing the high-strength epoxy resin repair mortar according to claim 2, wherein the method comprises the following steps: the solvent recovery process of step S3 includes the following steps,
cooling the recovered solvent at 25-30 ℃, adding potassium fluoride, stirring and heating at 170-180 ℃, adding chloroethanol, stirring for 3-4h, uniformly stirring, cooling at 0-3 ℃, adding pyridine, stirring for 3-3.5h, and adding the obtained product into the component A.
4. The method for preparing high-strength epoxy resin repair mortar according to claim 3, wherein the method comprises the following steps: the solvent recovery treatment operation needs to be performed under a nitrogen atmosphere.
5. The repair mortar prepared by the method for preparing a high-strength epoxy resin repair mortar according to any one of claims 1 to 4, wherein: the repair mortar comprises a component A and a curing agent, wherein the component A and the curing agent are mixed according to the mass ratio of 3-5: 1;
the component A is prepared from the following raw materials, by weight, 50-60 parts of modified epoxy resin, 40-50 parts of quartz sand and 10-15 parts of glass fiber.
6. The high-strength epoxy resin repair mortar of claim 5, wherein: the organic silicon monomer is one or a mixture of two of monomethyloxytriethoxysilane and dimethyldiethoxysilane.
7. The high-strength epoxy resin repair mortar of claim 5, wherein: the solvent is a mixture of ethylene glycol, xylene and acetone;
the mass ratio of the ethylene glycol to the xylene to the acetone is 7:3: 1.
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