CN112321194A - Preparation method of high-temperature-resistant additive for concrete - Google Patents
Preparation method of high-temperature-resistant additive for concrete Download PDFInfo
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G77/48—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
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Abstract
The invention discloses a preparation method of a high-temperature resistant additive for concrete, which comprises the following steps: firstly, weighing the following raw materials in parts by weight: 6-10 parts of styrene butadiene rubber, 7-9 parts of polyethylene wax, 10-15 parts of petroleum resin, 10-12 parts of rosin resin, 10-15 parts of polyvinyl chloride resin, 10-20 parts of naphthenic oil, 6-10 parts of filler, 3-5 parts of hydrogel, 0.6-1 part of antioxidant and 9-11 parts of plasticizer; secondly, heating styrene butadiene rubber, polyethylene wax, petroleum resin, rosin resin, polyvinyl chloride resin and naphthenic oil to 200 ℃, and reacting for 20-30min to obtain a mixture A; thirdly, adding the filler, the hydrogel, the antioxidant and the plasticizer into the obtained mixture A, and then stirring for 30-50min at 100 ℃; cooling to room temperature to obtain the high-temperature resistant additive for concrete.
Description
Technical Field
The invention belongs to the technical field of building material preparation, and particularly relates to a preparation method of a high-temperature-resistant additive for concrete.
Background
The concrete additive is a plastic adhesive, its physical state changes with the change of temperature in a certain temperature range, and its chemical property does not change, and it is non-toxic, odourless and belongs to the environment-protecting type chemical product. The product is solid, so the product is convenient to package, transport and store, and has no solvent, pollution and toxicity; and the production process is simple, the added value is high, the bonding strength is high, the speed is high, and the like. Concrete additives have been widely used in various fields such as molding, joining, building materials, and the like. Concrete curing is a hydration exothermic process, which affects the use effect of the additive.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a preparation method of a high-temperature resistant additive for concrete.
The technical problems to be solved by the invention are as follows:
the concrete additive is generally a plastic adhesive, the physical state of the concrete additive changes along with the change of temperature in a certain temperature range, and the concrete curing is a hydration heat release process which influences the use effect of the additive.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a high-temperature resistant additive for concrete comprises the following steps:
firstly, weighing the following raw materials in parts by weight:
6-10 parts of styrene butadiene rubber, 7-9 parts of polyethylene wax, 10-15 parts of petroleum resin, 10-12 parts of rosin resin, 10-15 parts of polyvinyl chloride resin, 10-20 parts of naphthenic oil, 6-10 parts of filler, 3-5 parts of hydrogel, 0.6-1 part of antioxidant and 9-11 parts of plasticizer;
secondly, heating styrene butadiene rubber, polyethylene wax, petroleum resin, rosin resin, polyvinyl chloride resin and naphthenic oil to 200 ℃, and reacting for 20-30min to obtain a mixture A;
thirdly, adding the filler, the hydrogel, the antioxidant and the plasticizer into the obtained mixture A, and then stirring for 30-50min at 100 ℃; cooling to room temperature to obtain the high-temperature resistant additive for concrete.
Further, the antioxidant is one or more of 2, 6-tertiary butyl-4-methylphenol, bis (3, 5-tertiary butyl-4-hydroxyphenyl) thioether and dioctadecyl thiodipropionate which are mixed in any proportion; the plasticizer is di (2-ethylhexyl) phthalate and tricresyl phosphate according to the mass ratio of 1: 3-5, and mixing.
Further, the filler is prepared by the following steps:
step S11, mixing alkoxy silane monomers in proportion, adding the mixture into a three-neck flask, setting the temperature at 80 ℃ and the rotating speed at 200r/min, adding deionized water, stirring for 10-25min, then adding 10% boric acid, reacting for 10-20min, adding the rest boric acid, continuing to react for 3-4h, cooling to 70 ℃ after the reaction is finished, distilling the reaction liquid under reduced pressure, and removing water to obtain a polymer a;
step S12, mixing the polymer a and the dimethylbenzene until the polymer a is completely dissolved to obtain a solution b, adding epoxy resin into a four-neck flask, setting the temperature at 40 ℃ and the rotating speed at 400r/min, starting stirring, heating until the epoxy resin is completely dissolved, adding the solution b and a mixed solvent, then increasing the temperature to 150-;
step S13, mixing kaolin, carbamide and ethanol according to the mass ratio of 5: 8: 2, adding the mixture into a three-neck flask, performing ultrasonic treatment for 20-30min at the temperature of 60-70 ℃ and the frequency of 50-60kHz, keeping the temperature unchanged, stirring for 4-6h at the rotation speed of 600r/min to obtain pasty slurry, performing vacuum filtration on the pasty slurry to remove filtrate, washing a filter cake for three times by using deionized water at the temperature of 60 ℃, then washing for three times by using absolute ethyl alcohol, and drying the washed filter cake to constant weight at the temperature of 60 ℃ to obtain a base material;
and step S14, mixing the deionized water, the mixture c and the base material to prepare slurry, adjusting the pH value of the slurry to 9-10 by using sodium hydroxide, grinding the slurry to 500 meshes, adjusting the pH value of the slurry to 7 by using hydrochloric acid, adding alkylphenol ethoxylate and a silane coupling agent KH550, mixing, then carrying out vacuum filtration, and drying the obtained filter cake to constant weight to obtain the filler.
Further, in the step S11, the alkoxysilane monomer is methyl triethoxysilane, phenyl triethoxysilane, and dimethyl diethoxysilane in a mass ratio of 4-12: 3-15: 3, mixing, wherein the dosage ratio of the alkoxy silane monomer to the deionized water is 1-3 g: 100mL, wherein the using amount of boric acid is 7-13% of the total mass of the alkoxy silane monomers; in the step S12, the epoxy resin is one or two of epoxy resin E51 and epoxy resin E44 which are mixed in any proportion, and the mixed solvent is normal hexane and cyclohexanone according to the volume ratio of 1: 5, mixing the components; the dosage ratio of the polymer a, the dimethylbenzene, the epoxy resin and the mixed solvent is 2 g: 3mL of: 10 g: 6 mL; in the step S14, the dosage ratio of the deionized water to the mixture c to the base material to the alkylphenol polyoxyethylene ether to the silane coupling agent KH550 is 50 mL: 6 g: 13 g: 0.7 g: 0.5 g.
Reacting active hydroxyl on boric acid with reactive alkoxy in alkoxy silane, wherein a-B-O-bond in boric acid molecules is connected into a-Si-O-main chain to obtain a polymer a, and the boric acid is a Lewis acid and is a reactant in the reaction and has catalytic action on polymerization reaction; boric acid is trifunctional inorganic acid, more crosslinking points can be provided after the reaction polymerization reaction, simultaneously, more-B-O-Si-with excellent heat resistance is introduced, the main chain of the polymer a is firmer and not easy to break when being heated, the-Si-O-R in the polymer a can perform dealcoholization reaction with alcoholic hydroxyl in epoxy resin, the adhesive force of the epoxy resin is strong, the introduction of epoxy groups, and the epoxy resin and the polymer a are subjected to copolymerization condensation to prepare a mixture c, so that the heat resistance and the durability are improved. The base material is modified kaolin, carbamide is used as an intercalation agent to provide an embedding space for the mixture c, and on the other hand, the kaolin can be decomposed into water and metal oxide at high temperature and can play a role in flame retardance to a certain extent.
Further, the aerogel is prepared by the following steps:
step S21, mixing manganese sulfate monohydrate and deionized water to obtain a solution d, mixing potassium permanganate and deionized water to obtain a solution e, adding microcrystalline cellulose into the solution d, setting the temperature to be 30 ℃ and the rotating speed to be 300r/min, stirring for 30min, then dropwise adding the solution e into the solution d by using a constant-pressure dropping funnel, controlling the dropwise adding speed to be 1-3 drops/second, keeping the temperature and the rotating speed unchanged after the dropwise adding is completed, continuously stirring for 8h to obtain a mixed solution, centrifuging the obtained mixed solution at the rotating speed of 1000r/min for 20min, filtering, washing by using deionized water, and drying at the temperature of 60 ℃ to constant weight to obtain a solid f;
and step S22, mixing sodium alginate and deionized water, adding solid f and calcium carbonate, uniformly mixing, adding glucolactone, and stirring at the set temperature of 30 ℃ and the rotation speed of 500r/min for 30min to obtain the hydrogel.
Further, in the step S21, the concentration of the solution d is 0.005g/mL, the concentration of the solution e is 0.005g/mL, and the volume ratio of the solution d to the solution e is 1.5: 1; the dosage ratio of the microcrystalline cellulose to the solution d is 4g:150-160 mL; in the step S22, the mass ratio of the sodium alginate to the deionized water to the solid f to the calcium carbonate to the gluconolactone is 1: 100: 1-3: 1: 0.1-0.3.
The method comprises the steps of utilizing microcrystalline cellulose as a base material, utilizing potassium permanganate and potassium sulfate as raw materials to generate manganese dioxide which is in a nanometer level, then gradually gelatinizing ammonium alginate under the induction action of calcium ions, enabling the nano manganese dioxide to have a large specific surface area, enabling surface hydroxyl groups to be rich and enabling particle sizes to be small, fixing the microcrystalline cellulose and the manganese dioxide in the nano manganese dioxide to form uniformly dispersed hydrogel which has strong adsorption force and a high specific surface area, improving the strength of the hydrogel due to the existence of the microcrystalline cellulose, and improving the bonding strength of an additive and concrete due to the addition of the hydrogel according to the structural characteristics of the hydrogel.
The invention has the beneficial effects that:
reacting active hydroxyl on boric acid with reactive alkoxy in alkoxy silane, wherein a-B-O-bond in boric acid molecules is connected into a-Si-O-main chain to obtain a polymer a, and the boric acid is a Lewis acid and is a reactant in the reaction and has catalytic action on polymerization reaction; boric acid is trifunctional inorganic acid, more crosslinking points can be provided after the reaction polymerization reaction, simultaneously, more-B-O-Si-with excellent heat resistance is introduced, the main chain of the polymer a is firmer and not easy to break when being heated, the-Si-O-R in the polymer a can perform dealcoholization reaction with alcoholic hydroxyl in epoxy resin, the adhesive force of the epoxy resin is strong, the introduction of epoxy groups, and the epoxy resin and the polymer a are subjected to copolymerization condensation to prepare a mixture c, so that the heat resistance and the durability are improved. The base material is modified kaolin, carbamide is used as an intercalation agent to provide an embedding space for the mixture c, and on the other hand, the kaolin can be decomposed into water and metal oxide at high temperature and can play a role in flame retardance to a certain extent.
The method comprises the steps of utilizing microcrystalline cellulose as a base material, utilizing potassium permanganate and potassium sulfate as raw materials to generate manganese dioxide which is in a nanometer level, then gradually gelatinizing ammonium alginate under the induction action of calcium ions, enabling the nano manganese dioxide to have a large specific surface area, enabling surface hydroxyl groups to be rich and enabling particle sizes to be small, fixing the microcrystalline cellulose and the manganese dioxide in the nano manganese dioxide to form uniformly dispersed hydrogel which has strong adsorption force and a high specific surface area, improving the strength of the hydrogel due to the existence of the microcrystalline cellulose, and improving the bonding strength of an additive and concrete due to the addition of the hydrogel according to the structural characteristics of the hydrogel.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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
A preparation method of a high-temperature resistant additive for concrete comprises the following steps: firstly, weighing the following raw materials in parts by weight:
6 parts of styrene butadiene rubber, 7 parts of polyethylene wax, 10 parts of petroleum resin, 10 parts of rosin resin, 10 parts of polyvinyl chloride resin, 10 parts of naphthenic oil, 6 parts of filler, 3 parts of hydrogel, 0.6 part of antioxidant and 9 parts of plasticizer;
secondly, heating styrene butadiene rubber, polyethylene wax, petroleum resin, rosin resin, polyvinyl chloride resin and naphthenic oil to 200 ℃, and reacting for 20min to obtain a mixture A;
thirdly, adding the filler, the hydrogel, the antioxidant and the plasticizer into the obtained mixture A, and then stirring for 30min at 100 ℃; cooling to room temperature to obtain the high-temperature resistant additive for concrete.
Wherein the antioxidant is 2, 6-tertiary butyl-4-methylphenol; the plasticizer is di (2-ethylhexyl) phthalate and tricresyl phosphate according to the mass ratio of 1: 3, mixing.
Wherein the filler is prepared by the following steps:
step S11, mixing alkoxy silane monomers in proportion, adding the mixture into a three-neck flask, setting the temperature at 80 ℃ and the rotating speed at 200r/min, adding deionized water, stirring for 10min, then adding 10% boric acid, reacting for 10min, adding the rest boric acid, continuing to react for 3h, cooling to 70 ℃ after the reaction is finished, distilling the reaction liquid under reduced pressure, and removing water to obtain a polymer a;
step S12, mixing the polymer a and xylene until the polymer a is completely dissolved to obtain a solution b, adding epoxy resin into a four-neck flask, setting the temperature to be 40 ℃ and the rotating speed to be 400r/min, starting stirring, heating until the epoxy resin is completely dissolved, adding the solution b and a mixed solvent, then increasing the temperature to be 150 ℃, keeping the rotating speed unchanged, and continuing stirring for 4 hours to obtain a mixture c;
step S13, mixing kaolin, carbamide and ethanol according to the mass ratio of 5: 8: 2, adding the mixture into a three-neck flask, carrying out ultrasonic treatment for 20min at the temperature of 60 ℃ and the frequency of 50kHz, then keeping the temperature unchanged, stirring for 4h at the rotating speed of 600r/min to obtain pasty slurry, carrying out vacuum filtration on the pasty slurry, removing filtrate, washing a filter cake with deionized water at the temperature of 60 ℃ for three times, then washing the filter cake with absolute ethyl alcohol for three times, and drying the washed filter cake to constant weight at the temperature of 60 ℃ to obtain a base material;
and step S14, mixing the deionized water, the mixture c and the base material to prepare slurry, adjusting the pH value of the slurry to 9 by using sodium hydroxide, grinding the slurry to 500 meshes, adjusting the pH value of the slurry to 7 by using hydrochloric acid, adding alkylphenol ethoxylate and a silane coupling agent KH550, mixing, then carrying out vacuum filtration, and drying the obtained filter cake to constant weight to obtain the filler.
Wherein, the alkoxy silane monomer in the step S11 is methyl triethoxysilane, phenyl triethoxysilane and dimethyl diethoxy silane according to the mass ratio of 4: 3: 3, mixing, wherein the dosage ratio of the alkoxy silane monomer to the deionized water is 1 g: 100mL, wherein the using amount of boric acid is 7 percent of the total mass of the alkoxy silane monomers; in the step S12, the epoxy resin is epoxy resin E51, and the mixed solvent is n-hexane and cyclohexanone in a volume ratio of 1: 5, mixing the components; the dosage ratio of the polymer a, the dimethylbenzene, the epoxy resin and the mixed solvent is 2 g: 3mL of: 10 g: 6 mL; in the step S14, the dosage ratio of the deionized water to the mixture c to the base material to the alkylphenol polyoxyethylene ether to the silane coupling agent KH550 is 50 mL: 6 g: 13 g: 0.7 g: 0.5 g.
Wherein the aerogel is prepared by the following steps:
step S21, mixing manganese sulfate monohydrate and deionized water to obtain a solution d, mixing potassium permanganate and deionized water to obtain a solution e, adding microcrystalline cellulose into the solution d, setting the temperature to be 30 ℃ and the rotating speed to be 300r/min, stirring for 30min, then dropwise adding the solution e into the solution d by using a constant-pressure dropping funnel, controlling the dropwise adding speed to be 1 drop/sec, keeping the temperature and the rotating speed unchanged after the dropwise adding is completed, continuously stirring for 8h to obtain a mixed solution, centrifuging the obtained mixed solution at the rotating speed of 1000r/min for 20min, filtering, washing by using deionized water, and drying at the temperature of 60 ℃ to constant weight to obtain a solid f;
and step S22, mixing sodium alginate and deionized water, adding solid f and calcium carbonate, uniformly mixing, adding glucolactone, and stirring at the set temperature of 30 ℃ and the rotation speed of 500r/min for 30min to obtain the hydrogel.
Wherein the concentration of the solution d in the step S21 is 0.005g/mL, the concentration of the solution e is 0.005g/mL, and the volume ratio of the solution d to the solution e is 1.5: 1; the dosage ratio of the microcrystalline cellulose to the solution d is 4g:150 mL; in the step S22, the mass ratio of the sodium alginate to the deionized water to the solid f to the calcium carbonate to the gluconolactone is 1: 100: 1: 1: 0.1.
example 2
A preparation method of a high-temperature resistant additive for concrete comprises the following steps: firstly, weighing the following raw materials in parts by weight:
8 parts of styrene butadiene rubber, 8 parts of polyethylene wax, 12 parts of petroleum resin, 11 parts of rosin resin, 12 parts of polyvinyl chloride resin, 15 parts of naphthenic oil, 8 parts of filler, 4 parts of hydrogel, 0.8 part of antioxidant and 10 parts of plasticizer;
secondly, heating styrene butadiene rubber, polyethylene wax, petroleum resin, rosin resin, polyvinyl chloride resin and naphthenic oil to 200 ℃, and reacting for 25min to obtain a mixture A;
thirdly, adding the filler, the hydrogel, the antioxidant and the plasticizer into the obtained mixture A, and then stirring for 40min at 100 ℃; cooling to room temperature to obtain the high-temperature resistant additive for concrete.
Wherein the antioxidant is dioctadecyl thiodipropionate; the plasticizer is di (2-ethylhexyl) phthalate and tricresyl phosphate according to the mass ratio of 1: 4, mixing.
Wherein the filler is prepared by the following steps:
step S11, mixing alkoxy silane monomers in proportion, adding the mixture into a three-neck flask, setting the temperature at 80 ℃ and the rotating speed at 200r/min, adding deionized water, stirring for 18min, then adding 10% boric acid, reacting for 15min, adding the rest boric acid, continuing to react for 3.5h, cooling to 70 ℃ after the reaction is finished, distilling the reaction liquid under reduced pressure, and removing water to obtain a polymer a;
step S12, mixing the polymer a and xylene until the polymer a is completely dissolved to obtain a solution b, adding epoxy resin into a four-neck flask, setting the temperature to be 40 ℃ and the rotating speed to be 400r/min, starting stirring, heating until the epoxy resin is completely dissolved, adding the solution b and a mixed solvent, then increasing the temperature to be 155 ℃, keeping the rotating speed unchanged, and continuing stirring for 6 hours to obtain a mixture c;
step S13, mixing kaolin, carbamide and ethanol according to the mass ratio of 5: 8: 2, adding the mixture into a three-neck flask, carrying out ultrasonic treatment for 25min at the temperature of 65 ℃ and the frequency of 55kHz, keeping the temperature unchanged, stirring for 5h at the rotating speed of 600r/min to obtain pasty slurry, carrying out vacuum filtration on the pasty slurry, removing filtrate, washing a filter cake with deionized water at 60 ℃ for three times, then washing the filter cake with absolute ethyl alcohol for three times, and drying the washed filter cake to constant weight at 60 ℃ to obtain a base material;
and step S14, mixing the deionized water, the mixture c and the base material to prepare slurry, adjusting the pH value of the slurry to 9 by using sodium hydroxide, grinding the slurry to 500 meshes, adjusting the pH value of the slurry to 7 by using hydrochloric acid, adding alkylphenol ethoxylate and a silane coupling agent KH550, mixing, then carrying out vacuum filtration, and drying the obtained filter cake to constant weight to obtain the filler.
Wherein, the alkoxy silane monomer in the step S11 is methyl triethoxysilane, phenyl triethoxysilane and dimethyl diethoxy silane according to the mass ratio of 8: 9: 3, mixing, wherein the dosage ratio of the alkoxy silane monomer to the deionized water is 2 g: 100mL, wherein the using amount of boric acid is 10 percent of the total mass of the alkoxy silane monomers; in the step S12, the epoxy resin is epoxy resin E51 and epoxy resin E44 according to the mass ratio of 1: 1, mixing, wherein the mixed solvent is n-hexane and cyclohexanone according to a volume ratio of 1: 5, mixing the components; the dosage ratio of the polymer a, the dimethylbenzene, the epoxy resin and the mixed solvent is 2 g: 3mL of: 10 g: 6 mL; in the step S14, the dosage ratio of the deionized water to the mixture c to the base material to the alkylphenol polyoxyethylene ether to the silane coupling agent KH550 is 50 mL: 6 g: 13 g: 0.7 g: 0.5 g.
Wherein the aerogel is prepared by the following steps:
step S21, mixing manganese sulfate monohydrate and deionized water to obtain a solution d, mixing potassium permanganate and deionized water to obtain a solution e, adding microcrystalline cellulose into the solution d, setting the temperature to be 30 ℃ and the rotating speed to be 300r/min, stirring for 30min, then dropwise adding the solution e into the solution d by using a constant-pressure dropping funnel, controlling the dropwise adding speed to be 2 drops/sec, keeping the temperature and the rotating speed unchanged after dropwise adding is completed, continuously stirring for 8h to obtain a mixed solution, centrifuging the obtained mixed solution at the rotating speed of 1000r/min for 20min, filtering, washing by using deionized water, and drying at the temperature of 60 ℃ to constant weight to obtain a solid f;
and step S22, mixing sodium alginate and deionized water, adding solid f and calcium carbonate, uniformly mixing, adding glucolactone, and stirring at the set temperature of 30 ℃ and the rotation speed of 500r/min for 30min to obtain the hydrogel.
Wherein the concentration of the solution d in the step S21 is 0.005g/mL, the concentration of the solution e is 0.005g/mL, and the volume ratio of the solution d to the solution e is 1.5: 1; the dosage ratio of the microcrystalline cellulose to the solution d is 4g:155 mL; in the step S22, the mass ratio of the sodium alginate to the deionized water to the solid f to the calcium carbonate to the gluconolactone is 1: 100: 2: 1: 0.2.
example 3
A preparation method of a high-temperature resistant additive for concrete comprises the following steps: firstly, weighing the following raw materials in parts by weight:
10 parts of styrene butadiene rubber, 9 parts of polyethylene wax, 15 parts of petroleum resin, 12 parts of rosin resin, 15 parts of polyvinyl chloride resin, 20 parts of naphthenic oil, 10 parts of filler, 5 parts of hydrogel, 1 part of antioxidant and 11 parts of plasticizer;
secondly, heating styrene butadiene rubber, polyethylene wax, petroleum resin, rosin resin, polyvinyl chloride resin and naphthenic oil to 200 ℃, and reacting for 30min to obtain a mixture A;
thirdly, adding the filler, the hydrogel, the antioxidant and the plasticizer into the obtained mixture A, and then stirring for 50min at 100 ℃; cooling to room temperature to obtain the high-temperature resistant additive for concrete.
Wherein the antioxidant is bis (3, 5-tertiary butyl-4-hydroxyphenyl) thioether; the plasticizer is di (2-ethylhexyl) phthalate and tricresyl phosphate according to the mass ratio of 1: and 5, mixing.
Wherein the filler is prepared by the following steps:
step S11, mixing alkoxy silane monomers in proportion, adding the mixture into a three-neck flask, setting the temperature at 80 ℃ and the rotating speed at 200r/min, adding deionized water, stirring for 25min, then adding 10% boric acid, reacting for 20min, adding the rest boric acid, continuing to react for 4h, cooling to 70 ℃ after the reaction is finished, distilling the reaction liquid under reduced pressure, and removing water to obtain a polymer a;
step S12, mixing the polymer a and xylene until the polymer a is completely dissolved to obtain a solution b, adding epoxy resin into a four-neck flask, setting the temperature to be 40 ℃ and the rotating speed to be 400r/min, starting stirring, heating until the epoxy resin is completely dissolved, adding the solution b and a mixed solvent, then increasing the temperature to be 160 ℃, keeping the rotating speed unchanged, and continuing stirring for 8 hours to obtain a mixture c;
step S13, mixing kaolin, carbamide and ethanol according to the mass ratio of 5: 8: 2, adding the mixture into a three-neck flask, carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ and the frequency of 60kHz, then keeping the temperature unchanged, stirring for 6h at the rotating speed of 600r/min to obtain pasty slurry, carrying out vacuum filtration on the pasty slurry, removing filtrate, washing a filter cake with deionized water at the temperature of 60 ℃ for three times, then washing the filter cake with absolute ethyl alcohol for three times, and drying the washed filter cake to constant weight at the temperature of 60 ℃ to obtain a base material;
and step S14, mixing the deionized water, the mixture c and the base material to prepare slurry, adjusting the pH value of the slurry to 10 by using sodium hydroxide, grinding the slurry to 500 meshes, adjusting the pH value of the slurry to 7 by using hydrochloric acid, adding alkylphenol ethoxylates and a silane coupling agent KH550, mixing, then carrying out vacuum filtration, and drying the obtained filter cake to constant weight to obtain the filler.
Wherein, the alkoxy silane monomer in the step S11 is methyl triethoxysilane, phenyl triethoxysilane and dimethyl diethoxy silane according to the mass ratio of 12: 15: 3, mixing, wherein the dosage ratio of the alkoxy silane monomer to the deionized water is 3 g: 100mL, wherein the using amount of boric acid is 13 percent of the total mass of the alkoxy silane monomers; in the step S12, the epoxy resin is epoxy resin E44, and the mixed solvent is n-hexane and cyclohexanone in a volume ratio of 1: 5, mixing the components; the dosage ratio of the polymer a, the dimethylbenzene, the epoxy resin and the mixed solvent is 2 g: 3mL of: 10 g: 6 mL; in the step S14, the dosage ratio of the deionized water to the mixture c to the base material to the alkylphenol polyoxyethylene ether to the silane coupling agent KH550 is 50 mL: 6 g: 13 g: 0.7 g: 0.5 g.
Wherein the aerogel is prepared by the following steps:
step S21, mixing manganese sulfate monohydrate and deionized water to obtain a solution d, mixing potassium permanganate and deionized water to obtain a solution e, adding microcrystalline cellulose into the solution d, setting the temperature to be 30 ℃ and the rotating speed to be 300r/min, stirring for 30min, then dropwise adding the solution e into the solution d by using a constant-pressure dropping funnel, controlling the dropwise adding speed to be 3 drops/sec, keeping the temperature and the rotating speed unchanged after the dropwise adding is completed, continuously stirring for 8h to obtain a mixed solution, centrifuging the obtained mixed solution at the rotating speed of 1000r/min for 20min, filtering, washing by using deionized water, and drying at the temperature of 60 ℃ to constant weight to obtain a solid f;
and step S22, mixing sodium alginate and deionized water, adding solid f and calcium carbonate, uniformly mixing, adding glucolactone, and stirring at the set temperature of 30 ℃ and the rotation speed of 500r/min for 30min to obtain the hydrogel.
Wherein the concentration of the solution d in the step S21 is 0.005g/mL, the concentration of the solution e is 0.005g/mL, and the volume ratio of the solution d to the solution e is 1.5: 1; the dosage ratio of the microcrystalline cellulose to the solution d is 4g:160 mL; in the step S22, the mass ratio of the sodium alginate to the deionized water to the solid f to the calcium carbonate to the gluconolactone is 1: 100: 3: 1: 0.3.
comparative example 1
The comparative example is a common high-temperature resistant additive for concrete on the market.
The additives of examples 1-3 and comparative example 1 were subjected to performance tests, the results of which are shown below:
TABLE 1
| Examples | Softening point/. degree.C | High temperature resistance/deg.C | Peeling temperature/. degree.C |
| Example 1 | 136 | 140 | 91 |
| Example 2 | 138 | 145 | 93 |
| Example 3 | 135 | 142 | 95 |
| Comparative example 1 | 90 | 100 | 72 |
As can be seen from table 1 above, the high temperature resistant additive for concrete prepared by the present invention has better high temperature resistance than the common additives on the market.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (6)
1. A preparation method of a high-temperature resistant additive for concrete is characterized by comprising the following steps: firstly, weighing the following raw materials in parts by weight:
6-10 parts of styrene butadiene rubber, 7-9 parts of polyethylene wax, 10-15 parts of petroleum resin, 10-12 parts of rosin resin, 10-15 parts of polyvinyl chloride resin, 10-20 parts of naphthenic oil, 6-10 parts of filler, 3-5 parts of hydrogel, 0.6-1 part of antioxidant and 9-11 parts of plasticizer;
secondly, heating styrene butadiene rubber, polyethylene wax, petroleum resin, rosin resin, polyvinyl chloride resin and naphthenic oil to 200 ℃, and reacting for 20-30min to obtain a mixture A;
thirdly, adding the filler, the hydrogel, the antioxidant and the plasticizer into the obtained mixture A, and then stirring for 30-50min at 100 ℃; cooling to room temperature to obtain the high-temperature resistant additive for concrete.
2. The method for preparing the high temperature resistant additive for concrete according to claim 1, wherein the antioxidant is one or more of 2, 6-tertiary butyl-4-methylphenol, bis (3, 5-tertiary butyl-4-hydroxyphenyl) sulfide and dioctadecyl thiodipropionate mixed in any proportion; the plasticizer is di (2-ethylhexyl) phthalate and tricresyl phosphate according to the mass ratio of 1: 3-5, and mixing.
3. The method for preparing the high temperature resistant additive for concrete according to claim 1, wherein the filler is prepared by the following steps:
step S11, mixing alkoxy silane monomers in proportion, adding the mixture into a three-neck flask, setting the temperature at 80 ℃ and the rotating speed at 200r/min, adding deionized water, stirring for 10-25min, then adding 10% boric acid, reacting for 10-20min, adding the rest boric acid, continuing to react for 3-4h, cooling to 70 ℃ after the reaction is finished, distilling the reaction liquid under reduced pressure, and removing water to obtain a polymer a;
step S12, mixing the polymer a and the dimethylbenzene until the polymer a is completely dissolved to obtain a solution b, adding epoxy resin into a four-neck flask, setting the temperature at 40 ℃ and the rotating speed at 400r/min, starting stirring, heating until the epoxy resin is completely dissolved, adding the solution b and a mixed solvent, then increasing the temperature to 150-;
step S13, mixing kaolin, carbamide and ethanol according to the mass ratio of 5: 8: 2, adding the mixture into a three-neck flask, performing ultrasonic treatment for 20-30min at the temperature of 60-70 ℃ and the frequency of 50-60kHz, keeping the temperature unchanged, stirring for 4-6h at the rotation speed of 600r/min to obtain pasty slurry, performing vacuum filtration on the pasty slurry to remove filtrate, washing a filter cake for three times by using deionized water at the temperature of 60 ℃, then washing for three times by using absolute ethyl alcohol, and drying the washed filter cake to constant weight at the temperature of 60 ℃ to obtain a base material;
and step S14, mixing the deionized water, the mixture c and the base material to prepare slurry, adjusting the pH value of the slurry to 9-10 by using sodium hydroxide, grinding the slurry to 500 meshes, adjusting the pH value of the slurry to 7 by using hydrochloric acid, adding alkylphenol ethoxylate and a silane coupling agent KH550, mixing, then carrying out vacuum filtration, and drying the obtained filter cake to constant weight to obtain the filler.
4. The method for preparing the high temperature resistant additive for concrete according to claim 3, wherein the alkoxysilane monomer in step S11 is methyl triethoxysilane, phenyl triethoxysilane, and dimethyl diethoxysilane at a mass ratio of 4-12: 3-15: 3, mixing, wherein the dosage ratio of the alkoxy silane monomer to the deionized water is 1-3 g: 100mL, wherein the using amount of boric acid is 7-13% of the total mass of the alkoxy silane monomers; in the step S12, the epoxy resin is one or two of epoxy resin E51 and epoxy resin E44 which are mixed in any proportion, and the mixed solvent is normal hexane and cyclohexanone according to the volume ratio of 1: 5, mixing the components; the dosage ratio of the polymer a, the dimethylbenzene, the epoxy resin and the mixed solvent is 2 g: 3mL of: 10 g: 6 mL; in the step S14, the dosage ratio of the deionized water to the mixture c to the base material to the alkylphenol polyoxyethylene ether to the silane coupling agent KH550 is 50 mL: 6 g: 13 g: 0.7 g: 0.5 g.
5. The method for preparing the high temperature resistant additive for concrete according to claim 1, wherein the aerogel is prepared by the following steps:
step S21, mixing manganese sulfate monohydrate and deionized water to obtain a solution d, mixing potassium permanganate and deionized water to obtain a solution e, adding microcrystalline cellulose into the solution d, setting the temperature to be 30 ℃ and the rotating speed to be 300r/min, stirring for 30min, then dropwise adding the solution e into the solution d by using a constant-pressure dropping funnel, controlling the dropwise adding speed to be 1-3 drops/second, keeping the temperature and the rotating speed unchanged after the dropwise adding is completed, continuously stirring for 8h to obtain a mixed solution, centrifuging the obtained mixed solution at the rotating speed of 1000r/min for 20min, filtering, washing by using deionized water, and drying at the temperature of 60 ℃ to constant weight to obtain a solid f;
and step S22, mixing sodium alginate and deionized water, adding solid f and calcium carbonate, uniformly mixing, adding glucolactone, and stirring at the set temperature of 30 ℃ and the rotation speed of 500r/min for 30min to obtain the hydrogel.
6. The method as claimed in claim 5, wherein the concentration of solution d in step S21 is 0.005g/mL, the concentration of solution e is 0.005g/mL, and the volume ratio of solution d to solution e is 1.5: 1; the dosage ratio of the microcrystalline cellulose to the solution d is 4g:150-160 mL; in the step S22, the mass ratio of the sodium alginate to the deionized water to the solid f to the calcium carbonate to the gluconolactone is 1: 100: 1-3: 1: 0.1-0.3.
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| CN114702277A (en) * | 2022-03-18 | 2022-07-05 | 石家庄市易达恒联路桥材料有限公司 | Prestressed duct grouting material and preparation method thereof |
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