CN112852018A - Water-soluble methyl silane environment-friendly asphalt separant - Google Patents

Water-soluble methyl silane environment-friendly asphalt separant Download PDF

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CN112852018A
CN112852018A CN202110042104.9A CN202110042104A CN112852018A CN 112852018 A CN112852018 A CN 112852018A CN 202110042104 A CN202110042104 A CN 202110042104A CN 112852018 A CN112852018 A CN 112852018A
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stirring
temperature
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reaction kettle
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秦敏
鹿亚东
张丽娟
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Fuyang Luxing Highway Engineering Testing Co ltd
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Fuyang Luxing Highway Engineering Testing Co ltd
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    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/5403—Silicon-containing compounds containing no other elements than carbon or hydrogen
    • 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
    • C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
    • C08F212/02—Monomers containing only one unsaturated aliphatic radical
    • C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F212/06—Hydrocarbons
    • C08F212/08—Styrene
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
    • C08L25/02—Homopolymers or copolymers of hydrocarbons
    • C08L25/04—Homopolymers or copolymers of styrene
    • C08L25/08—Copolymers of styrene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L89/00—Compositions of proteins; Compositions of derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation

Abstract

The invention discloses a water-soluble methyl silane environment-friendly asphalt separant, which comprises the following raw materials in parts by weight: 3-5 parts of methyl silane, 8-10 parts of kelp extract, 0.2-0.5 part of polyethylene glycol 20000, 4-6 parts of peregal, 1-3 parts of sodium aminotriacetate, 0.1-0.3 part of gelatin and 0.2-0.5 part of anti-aging agent; the electron cloud density on the oxygen atom on the anti-aging agent molecule is far greater than the electron cloud density on the nitrogen atom of the triazole ring when the anti-aging agent is illuminated, so that the anti-aging agent becomes strong alkaline, the electron density is shifted to the nitrogen atom from the oxygen atom after light absorption, so that the phenol structure in the molecule is more acidic, the nitrogen atom is more alkaline, the proton is quickly shifted to the nitrogen atom to form a tautomer, the tautomer is unstable, the light energy is converted into the heat energy to return to the stable ground state again, and further, the isolating agent is prevented from being oxidized, and the asphalt is prevented from being adhered to a processing or construction appliance.

Description

Water-soluble methyl silane environment-friendly asphalt separant
Technical Field
The invention relates to the field of asphalt preparation, and particularly relates to a water-soluble methyl silane environment-friendly asphalt separant.
Background
In the construction process of the asphalt pavement, rolling is the last procedure, the mechanical property and the functional characteristic of the asphalt concrete pavement are directly influenced by the quality of the rolling effect, high-quality rolling can ensure that the asphalt pavement layer achieves high compaction degree and has good balance degree, the service life of the pavement meets or exceeds the design requirement, and the isolating agent is used in the construction process for preventing and reducing the bonding of the asphalt mixture with transport vehicles and road roller mechanical equipment.
The existing asphalt isolation is used, the problem of viscosity still occurs when asphalt is processed and constructed, part of asphalt can be adhered to a processing or construction appliance and is illuminated in the processing process, oxidation can occur to reduce the effect of the isolating agent, and then a large amount of adhesion phenomena occur to the asphalt.
Disclosure of Invention
The invention aims to provide a water-soluble methyl silane environment-friendly asphalt separant.
The technical problems to be solved by the invention are as follows:
the existing asphalt isolation is used, the problem of viscosity still occurs when asphalt is processed and constructed, part of asphalt can be adhered to a processing or construction appliance and is illuminated in the processing process, oxidation can occur to reduce the effect of the isolating agent, and then a large amount of adhesion phenomena occur to the asphalt.
The purpose of the invention can be realized by the following technical scheme:
a water-soluble methyl silane environment-friendly asphalt separant comprises the following raw materials in parts by weight: 3-5 parts of methyl silane, 8-10 parts of kelp extract, 0.2-0.5 part of polyethylene glycol 20000, 4-6 parts of peregal, 1-3 parts of sodium aminotriacetate, 0.1-0.3 part of gelatin and 0.2-0.5 part of anti-aging agent;
the asphalt separant is prepared by the following steps:
step S1: adding methylsilane, herba Zosterae Marinae extract and polyethylene glycol 20000 into a stirring kettle, stirring at rotation speed of 300-500r/min and temperature of 60-70 deg.C for 10-15min to obtain a mixture;
step S2: adding peregal, sodium aminotriacetate and gelatin into a stirring kettle, stirring for 15-20min at the rotation speed of 200-800 r/min, adding the mixture and an anti-aging agent, stirring for 1-1.5h at the rotation speed of 500-800r/min, and adjusting the pH value to 6.5-7.5 to obtain the asphalt separant.
Further, the anti-aging agent is prepared by the following steps:
step A1: adding a sulfuric acid solution and deionized water into a reaction kettle, stirring and adding o-nitroaniline at the rotation speed of 150 plus 200r/min and the temperature of 3-5 ℃, dropwise adding a sodium nitrate solution for 0.5-0.8h after stirring for 10-15min, continuously stirring for 1-1.5h after dropwise adding is finished, adding p-methylphenol, continuously stirring for 3-5min, adjusting the pH value of the reaction solution to 7-9, continuously stirring for 2-3h, adding ethanol, a sodium hydroxide solution and a glucose solution, reacting for 1-1.5h at the temperature of 40-50 ℃, adding zinc powder, continuously reacting for 0.5-0.8h at the temperature of 85-90 ℃ to prepare an intermediate 1, and mixing the intermediate 1, nitrogen-succinimide, benzoyl peroxide bromide, bromine, and glucose to obtain an intermediate 1, Adding carbon tetrachloride into a reaction kettle, reacting for 8-10h at the temperature of 80-90 ℃ to obtain an intermediate 2, adding the intermediate 2, a potassium carbonate solution and tetraethylammonium bromide into the reaction kettle, and performing reflux reaction for 1-1.5h at the temperature of 120-130 ℃ to obtain an intermediate 3;
the reaction process is as follows:
Figure BDA0002896309710000021
Figure BDA0002896309710000031
step A2: adding diphenylamine, deionized water and concentrated hydrochloric acid into a reaction kettle, adding acetic anhydride and a sodium acetate solution under the conditions of a rotation speed of 200-;
the reaction process is as follows:
Figure BDA0002896309710000032
Figure BDA0002896309710000041
step A3: adding the intermediate 6, ethanol and concentrated sulfuric acid into a reaction kettle, performing reflux reaction at the rotation speed of 150-, adjusting the pH value of the reaction solution to 8, adding glacial acetic acid, and uniformly mixing to obtain an intermediate 10;
the reaction process is as follows:
Figure BDA0002896309710000042
Figure BDA0002896309710000051
step A4: dissolving cyanuric chloride in acetone, adding an intermediate 10, reacting for 5-6h at the rotation speed of 200-50 ℃ at 300r/min to obtain an intermediate 11, adding the intermediate 11, chlorobenzene and aluminum trichloride into a reaction kettle, stirring and adding magnesium powder at the rotation speed of 150-200r/min and the temperature of 3-5 ℃, stirring for 15-30min, adding toluene at the temperature of 0-3 ℃, stirring for 1-2h, continuously stirring for 10-15h at the temperature of 20-25 ℃, adding resorcinol, and reacting for 4-6h at the temperature of 80-90 ℃ to obtain an intermediate 12;
the reaction process is as follows:
Figure BDA0002896309710000052
Figure BDA0002896309710000061
step A5: adding the intermediate 12, 3-bromopropylene, sodium bicarbonate and acetone into a reaction kettle, performing reflux reaction for 6-8h at the temperature of 60-65 ℃ to obtain an intermediate 13, adding the intermediate 13, styrene and tetrahydrofuran into the reaction kettle, adding azobisisobutyronitrile at the rotation speed of 200-300r/min at the temperature of 70-80 ℃ to react for 3-4h, and precipitating with petroleum ether to obtain the anti-aging agent.
The reaction process is as follows:
Figure BDA0002896309710000062
further, the mass ratio of the sulfuric acid solution, the o-nitroaniline, the sodium nitrate solution, the p-methylphenol, the ethanol, the sodium hydroxide solution, the glucose solution and the zinc powder in the step A1 is 13.5g to 30.6g to 20g to 6.48g to 10mL to 10g to 15g to 1.3g, the mass fraction of the sulfuric acid solution is 98%, the mass fraction of the sodium nitrate solution is 30%, the mass fraction of the sodium hydroxide solution is 20%, the mass fraction of the glucose solution is 28.5%, the mass ratio of the intermediate 1, the nitrogen-bromosuccinimide, the benzoyl peroxide and the carbon tetrachloride is 0.15mol to 0.3g to 200mL, the mass ratio of the intermediate 2, the potassium carbonate solution and the tetraethylammonium bromide is 5g to 80mL to 2mL, and the mass fraction of the potassium carbonate solution is 12%.
Further, the dosage ratio of the diphenylamine, the deionized water, the concentrated hydrochloric acid, the acetic anhydride and the sodium acetate solution in the step A2 is 3.5g:90mL:4mL:6mL:12mL, the mass fraction of the concentrated hydrochloric acid is 25%, the dosage molar ratio of the intermediate 4 to the liquid-state methane chloride is 1:2, the dosage of the aluminum trichloride is 5-8% of the mass of the intermediate 4, the dosage ratio of the intermediate 5, the magnesium sulfate, the deionized water and the potassium permanganate solution is 3.5g:10g:175mL:50mL, and the mass fraction of the potassium permanganate solution is 23%.
Further, the molar ratio of the intermediate 6 to ethanol in the step A3 is 1:1, the amount of concentrated sulfuric acid is 20% of the mass of the intermediate 6, the mass fraction of concentrated sulfuric acid is 95%, the amount ratio of the intermediate 7, the intermediate 3, dibutyltin oxide and o-dichlorobenzene is 0.01mol:0.01mol:0.1g:6mL, the amount ratio of the intermediate 8, sulfur and iodine is 125mmol:250mmol:0.47mmol, the amount ratio of the intermediate 9 to hydrochloric acid solution is 1g:5mL, the mass fraction of hydrochloric acid solution is 18%, and the amount of glacial acetic acid is 3% of the total volume of the reaction solution.
Further, the molar ratio of the cyanuric chloride to the intermediate 10 in the step A4 is 1:1, and the molar ratio of the intermediate 11, chlorobenzene, aluminum trichloride, magnesium powder, toluene and resorcinol is 0.1mol:100mL:0.25mol:1g:20g:0.13 mol.
Further, the molar ratio of the intermediate 12, the 3-bromopropylene and the sodium bicarbonate in the step A5 is 1:1:1, the molar ratio of the intermediate 13 to the styrene is 1:71, and the amount of the azobisisobutyronitrile is 1-1.2% of the mass sum of the intermediate 13 and the styrene.
The invention has the beneficial effects that: the invention prepares an anti-aging agent in the process of preparing a water-soluble methyl silane environment-friendly asphalt separant, the anti-aging agent and o-nitroaniline are taken as raw materials to be processed to form diazotization solution, the diazotization solution is coupled with p-methylphenol and then reduced to prepare an intermediate 1, the intermediate 1 is reacted with nitrogen-bromosuccinimide to prepare an intermediate 2, the intermediate 2 is processed by potassium carbonate solution and tetraethylammonium bromide to prepare an intermediate 3, phenylenediamine is processed to prepare an intermediate 4, the intermediate 4 is reacted with monochloro methane to prepare an intermediate 5, the intermediate 5 is oxidized by potassium permanganate to prepare an intermediate 6, the intermediate 6 and ethanol are esterified to prepare an intermediate 7, the intermediate 7 and the intermediate 3 are subjected to ester exchange reaction to prepare an intermediate 8, the intermediate 8 is reacted with sulfur, preparing an intermediate 9, deprotecting the intermediate 9 to prepare an intermediate 10, reacting the intermediate 10 with cyanuric chloride at two chlorine atom sites on the cyanuric chloride under temperature control to prepare an intermediate 11, reacting the intermediate 11 with resorcinol to prepare an intermediate 12, reacting the intermediate 12 with 3-bromopropylene to prepare an intermediate 13, and polymerizing the intermediate 13 with styrene to prepare the anti-aging agent, wherein the anti-aging agent has a relatively large molecular weight and cannot volatilize when asphalt is paved, the electron cloud density on oxygen atoms on molecules of the anti-aging agent is far greater than that on nitrogen atoms of a triazole ring when the anti-aging agent is illuminated, so that the anti-aging agent becomes strongly basic, and the electron density is transferred from the oxygen atoms to the nitrogen atoms after the light absorption, so that the phenol structure in the molecules is more acidic, and the nitrogen atoms are more basic, the proton is rapidly transferred to the nitrogen atom to form tautomer, the tautomer is unstable, and the optical energy is converted into heat energy to return to a stable ground state, so that the separant is prevented from being oxidized, and the asphalt is prevented from being adhered to processing or construction equipment.
Detailed Description
The technical solutions in the embodiments of the present invention will be 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
A water-soluble methyl silane environment-friendly asphalt separant comprises the following raw materials in parts by weight: 3 parts of methylsilane, 8 parts of kelp extract, 0.2 part of polyethylene glycol 20000, 4 parts of peregal, 1 part of sodium aminotriacetate, 0.1 part of gelatin and 0.2 part of anti-aging agent;
the asphalt separant is prepared by the following steps:
step S1: adding methylsilane, herba Zosterae Marinae extract and polyethylene glycol 20000 into a stirring kettle, stirring at rotation speed of 300r/min and temperature of 60 deg.C for 10min to obtain a mixture;
step S2: adding peregal, sodium aminotriacetate and gelatin into a stirring kettle, stirring for 15min at the rotation speed of 200r/min, adding the mixture and an anti-aging agent, stirring for 1h at the rotation speed of 500r/min, and adjusting the pH value to 6.5 to obtain the asphalt separant.
The anti-aging agent is prepared by the following steps:
step A1: adding a sulfuric acid solution and deionized water into a reaction kettle, stirring and adding o-nitroaniline under the conditions that the rotating speed is 150r/min and the temperature is 3 ℃, stirring for 10min, dropwise adding a sodium nitrate solution for 0.5h, continuously stirring for 1h after dropwise adding is finished, adding p-methylphenol, continuously stirring for 3min, adjusting the pH value of a reaction solution to 7, continuously stirring for 2h, adding ethanol, a sodium hydroxide solution and a glucose solution, reacting for 1h under the condition that the temperature is 40 ℃, adding zinc powder, continuously reacting for 0.5h under the condition that the temperature is 85 ℃ to prepare an intermediate 1, adding the intermediate 1, nitrogen-bromosuccinimide, benzoyl peroxide and carbon tetrachloride into the reaction kettle, reacting for 8h under the condition that the temperature is 80 ℃ to prepare an intermediate 2, and adding a potassium carbonate solution, Adding tetraethylammonium bromide into a reaction kettle, and performing reflux reaction for 1h at the temperature of 120 ℃ to prepare an intermediate 3;
step A2: adding diphenylamine, deionized water and concentrated hydrochloric acid into a reaction kettle, adding acetic anhydride and a sodium acetate solution under the conditions of a rotation speed of 200r/min and a temperature of 50 ℃, stirring for 10min, cooling under the condition of an ice-water bath to prepare an intermediate 4, adding the intermediate 4, liquid-state chloromethane and aluminum trichloride into the reaction kettle, reacting for 3h under the condition of a temperature of 100 ℃ to prepare an intermediate 5, adding the intermediate 5, magnesium sulfate and deionized water into the reaction kettle, stirring and adding a potassium permanganate solution under the conditions of a rotation speed of 150r/min and a temperature of 80 ℃, and reacting for 3h to prepare an intermediate 6;
step A3: adding the intermediate 6, ethanol and concentrated sulfuric acid into a reaction kettle, performing reflux reaction at the rotation speed of 150r/min and the temperature of 80 ℃ to obtain an intermediate 7, adding the intermediate 7, the intermediate 3, dibutyltin oxide and o-dichlorobenzene into the reaction kettle, introducing nitrogen for protection, performing reaction for 6 hours at the rotation speed of 150r/min and the temperature of 150 ℃ to obtain an intermediate 8, adding the intermediate 8, sulfur and iodine into the reaction kettle, performing reaction at the rotation speed of 120r/min and the temperature of 180 ℃ until no hydrogen sulfide gas is generated, finishing the reaction to obtain an intermediate 9, adding the intermediate 9 and a hydrochloric acid solution into the reaction kettle, performing reflux for 30 minutes at the temperature of 110 ℃, adjusting the pH value of the reaction solution to be 8, adding glacial acetic acid, and uniformly mixing to obtain an intermediate 10;
step A4: dissolving cyanuric chloride in acetone, adding an intermediate 10, reacting for 5 hours at the rotation speed of 200r/min and the temperature of 40 ℃ to obtain an intermediate 11, adding the intermediate 11, chlorobenzene and aluminum trichloride into a reaction kettle, stirring and adding magnesium powder at the rotation speed of 150r/min and the temperature of 3 ℃, stirring for 15 minutes, adding toluene at the temperature of 0 ℃ and stirring for 1 hour, continuing to stir for 10 hours at the temperature of 20 ℃, adding resorcinol, and reacting for 4 hours at the temperature of 80 ℃ to obtain an intermediate 12;
step A5: adding the intermediate 12, 3-bromopropylene, sodium bicarbonate and acetone into a reaction kettle, performing reflux reaction for 6 hours at the temperature of 60 ℃ to obtain an intermediate 13, adding the intermediate 13, styrene and tetrahydrofuran into the reaction kettle, adding azobisisobutyronitrile at the rotation speed of 200r/min and the temperature of 70 ℃, reacting for 3 hours, and precipitating with petroleum ether to obtain the anti-aging agent.
Example 2
A water-soluble methyl silane environment-friendly asphalt separant comprises the following raw materials in parts by weight: 4 parts of methylsilane, 9 parts of kelp extract, 0.3 part of polyethylene glycol 20000, 5 parts of peregal, 2 parts of sodium aminotriacetate, 0.2 part of gelatin and 0.3 part of anti-aging agent;
the asphalt separant is prepared by the following steps:
step S1: adding methylsilane, herba Zosterae Marinae extract and polyethylene glycol 20000 into a stirring kettle, stirring at rotation speed of 300r/min and temperature of 70 deg.C for 10min to obtain a mixture;
step S2: adding peregal, sodium aminotriacetate and gelatin into a stirring kettle, stirring for 15min at the rotation speed of 300r/min, adding the mixture and an anti-aging agent, stirring for 1h at the rotation speed of 800r/min, and adjusting the pH value to 7.5 to obtain the asphalt separant.
The anti-aging agent is prepared by the following steps:
step A1: adding a sulfuric acid solution and deionized water into a reaction kettle, stirring and adding o-nitroaniline under the conditions that the rotating speed is 200r/min and the temperature is 3 ℃, stirring for 15min, dropwise adding a sodium nitrate solution for 0.5h, continuously stirring for 1.5h after dropwise adding is finished, adding p-methylphenol, continuously stirring for 3min, adjusting the pH value of a reaction solution to be 9, continuously stirring for 2h, adding ethanol, a sodium hydroxide solution and a glucose solution, reacting for 1h under the condition that the temperature is 50 ℃, adding zinc powder, continuously reacting for 0.5h under the condition that the temperature is 90 ℃ to prepare an intermediate 1, adding the intermediate 1, nitrogen-bromosuccinimide, benzoyl peroxide and carbon tetrachloride into the reaction kettle, reacting for 8h under the condition that the temperature is 90 ℃ to prepare an intermediate 2, adding a potassium carbonate solution, stirring for 15min, adding a sodium nitrate solution, stirring for 0.5h, stirring for 1h, and reacting for 8h under the condition that, Adding tetraethylammonium bromide into a reaction kettle, and performing reflux reaction for 1h at the temperature of 130 ℃ to prepare an intermediate 3;
step A2: adding diphenylamine, deionized water and concentrated hydrochloric acid into a reaction kettle, adding acetic anhydride and a sodium acetate solution under the conditions of a rotating speed of 300r/min and a temperature of 50 ℃, stirring for 15min, cooling under the condition of an ice-water bath to prepare an intermediate 4, adding the intermediate 4, liquid-state chloromethane and aluminum trichloride into the reaction kettle, reacting for 5h under the condition of a temperature of 100 ℃ to prepare an intermediate 5, adding the intermediate 5, magnesium sulfate and deionized water into the reaction kettle, stirring and adding a potassium permanganate solution under the conditions of a rotating speed of 150r/min and a temperature of 85 ℃, and reacting for 3h to prepare an intermediate 6;
step A3: adding the intermediate 6, ethanol and concentrated sulfuric acid into a reaction kettle, performing reflux reaction at the rotation speed of 200r/min and the temperature of 80 ℃ to obtain an intermediate 7, adding the intermediate 7, the intermediate 3, dibutyltin oxide and o-dichlorobenzene into the reaction kettle, introducing nitrogen for protection, performing reaction for 10 hours at the rotation speed of 200r/min and the temperature of 150 ℃ to obtain an intermediate 8, adding the intermediate 8, sulfur and iodine into the reaction kettle, performing reaction at the rotation speed of 120r/min and the temperature of 180 ℃ until no hydrogen sulfide gas is generated, finishing the reaction to obtain an intermediate 9, adding the intermediate 9 and a hydrochloric acid solution into the reaction kettle, performing reflux for 30 minutes at the temperature of 115 ℃, adjusting the pH value of the reaction solution to be 8, adding glacial acetic acid, and uniformly mixing to obtain an intermediate 10;
step A4: dissolving cyanuric chloride in acetone, adding an intermediate 10, reacting for 6 hours at the rotation speed of 300r/min and the temperature of 40 ℃ to obtain an intermediate 11, adding the intermediate 11, chlorobenzene and aluminum trichloride into a reaction kettle, stirring and adding magnesium powder at the rotation speed of 150r/min and the temperature of 5 ℃, stirring for 15 minutes, adding toluene at the temperature of 3 ℃, stirring for 1 hour, continuing stirring for 10 hours at the temperature of 25 ℃, adding resorcinol, and reacting for 4 hours at the temperature of 90 ℃ to obtain an intermediate 12;
step A5: adding the intermediate 12, 3-bromopropylene, sodium bicarbonate and acetone into a reaction kettle, performing reflux reaction for 6 hours at the temperature of 65 ℃ to obtain an intermediate 13, adding the intermediate 13, styrene and tetrahydrofuran into the reaction kettle, adding azobisisobutyronitrile at the rotation speed of 300r/min and the temperature of 70 ℃, reacting for 4 hours, and precipitating with petroleum ether to obtain the anti-aging agent.
Example 3
A water-soluble methyl silane environment-friendly asphalt separant comprises the following raw materials in parts by weight: 5 parts of methylsilane, 10 parts of kelp extract, 0.5 part of polyethylene glycol 20000, 6 parts of peregal, 3 parts of sodium aminotriacetate, 0.3 part of gelatin and 0.5 part of anti-aging agent;
the asphalt separant is prepared by the following steps:
step S1: adding methylsilane, herba Zosterae Marinae extract and polyethylene glycol 20000 into a stirring kettle, stirring at 70 deg.C at 500r/min for 15min to obtain a mixture;
step S2: adding peregal, sodium aminotriacetate and gelatin into a stirring kettle, stirring for 20min at the rotation speed of 300r/min, adding the mixture and an anti-aging agent, stirring for 1.5h at the rotation speed of 800r/min, and adjusting the pH value to 7.5 to obtain the asphalt separant.
The anti-aging agent is prepared by the following steps:
step A1: adding a sulfuric acid solution and deionized water into a reaction kettle, stirring and adding o-nitroaniline under the conditions that the rotating speed is 200r/min and the temperature is 5 ℃, stirring for 15min, dropwise adding a sodium nitrate solution for 0.8h, continuously stirring for 1.5h after dropwise adding is finished, adding p-methylphenol, continuously stirring for 5min, adjusting the pH value of a reaction solution to be 9, continuously stirring for 3h, adding ethanol, a sodium hydroxide solution and a glucose solution, reacting for 1.5h under the condition that the temperature is 50 ℃, adding zinc powder, continuously reacting for 0.8h under the condition that the temperature is 90 ℃ to prepare an intermediate 1, adding the intermediate 1, nitrogen-bromosuccinimide, benzoyl peroxide and carbon tetrachloride into the reaction kettle, reacting for 10h under the condition that the temperature is 90 ℃ to prepare an intermediate 2, and adding the intermediate 2, a potassium carbonate solution and a sodium chloride solution into the reaction kettle, Adding tetraethylammonium bromide into a reaction kettle, and carrying out reflux reaction for 1.5h at the temperature of 130 ℃ to prepare an intermediate 3;
step A2: adding diphenylamine, deionized water and concentrated hydrochloric acid into a reaction kettle, adding acetic anhydride and a sodium acetate solution under the conditions of a rotating speed of 300r/min and a temperature of 55 ℃, stirring for 15min, cooling under the condition of an ice-water bath to prepare an intermediate 4, adding the intermediate 4, liquid-state chloromethane and aluminum trichloride into the reaction kettle, reacting for 5h under the condition of a temperature of 105 ℃ to prepare an intermediate 5, adding the intermediate 5, magnesium sulfate and deionized water into the reaction kettle, stirring and adding a potassium permanganate solution under the conditions of a rotating speed of 200r/min and a temperature of 85 ℃, and reacting for 5h to prepare an intermediate 6;
step A3: adding the intermediate 6, ethanol and concentrated sulfuric acid into a reaction kettle, performing reflux reaction at the rotation speed of 200r/min and the temperature of 90 ℃ to obtain an intermediate 7, adding the intermediate 7, the intermediate 3, dibutyltin oxide and o-dichlorobenzene into the reaction kettle, introducing nitrogen for protection, reacting for 10 hours at the rotation speed of 150 plus 200r/min and the temperature of 160 ℃ to prepare an intermediate 8, adding the intermediate 8, sulfur and iodine into a reaction kettle, under the conditions that the rotating speed is 150r/min and the temperature is 180 ℃, the reaction is finished until no hydrogen sulfide gas is generated, an intermediate 9 is prepared, the intermediate 9 and hydrochloric acid solution are added into a reaction kettle, refluxing at 115 deg.C for 40min, adjusting pH to 8, adding glacial acetic acid, and mixing to obtain intermediate 10;
step A4: dissolving cyanuric chloride in acetone, adding an intermediate 10, reacting for 6 hours at the rotation speed of 300r/min and the temperature of 50 ℃ to obtain an intermediate 11, adding the intermediate 11, chlorobenzene and aluminum trichloride into a reaction kettle, stirring and adding magnesium powder at the rotation speed of 200r/min and the temperature of 5 ℃, stirring for 30 minutes, adding toluene at the temperature of 3 ℃, stirring for 2 hours, continuing stirring at the temperature of 25 ℃ for 15 hours, adding resorcinol, and reacting for 6 hours at the temperature of 90 ℃ to obtain an intermediate 12;
step A5: adding the intermediate 12, 3-bromopropylene, sodium bicarbonate and acetone into a reaction kettle, performing reflux reaction for 8 hours at the temperature of 65 ℃ to obtain an intermediate 13, adding the intermediate 13, styrene and tetrahydrofuran into the reaction kettle, adding azobisisobutyronitrile at the rotation speed of 300r/min and the temperature of 80 ℃, reacting for 4 hours, and precipitating with petroleum ether to obtain the anti-aging agent.
Comparative example
The comparative example is a common asphalt separant on the market.
The asphalt release agents prepared in examples 1 to 3 and comparative example were subjected to performance tests, and the test results are shown in table 1 below;
the asphalt separant prepared in examples 1 to 3 and the comparative example was added to asphalt mixtures to separate rubber wheels and separate vehicles for transporting asphalt mixtures, and whether the vehicles and rubber wheels adhered to the asphalt mixtures was observed.
The asphalt separants prepared in examples 1-3 and comparative examples were added to the asphalt mixture, and the asphalt mixture was irradiated at a wavelength of 340nm and an irradiation intensity of 0.68W/m2The stirring is carried out for 200, 300 and 500 hours while irradiating, and the stirring device is used for isolating the rubber wheels and isolating vehicles for transporting the asphalt mixture, and observing whether the asphalt mixture adheres to the transporting vehicles and the rubber wheels.
TABLE 1
Figure BDA0002896309710000141
Figure BDA0002896309710000151
From the above table 1, it can be seen that the separant prepared in examples 1 to 3, when added to an asphalt mixture, does not exhibit adhesion phenomenon when used for isolating rubber wheels and isolating asphalt mixture vehicles for transportation, and does not exhibit adhesion phenomenon after 500 hours of illumination, while the separant prepared in comparative example, when added to an asphalt mixture, exhibits a small amount of adhesion when used for isolating rubber wheels and isolating asphalt mixture vehicles for transportation, and exhibits a large amount of adhesion after 300 hours of illumination, and the invention has good aging resistance.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.

Claims (7)

1. A water-soluble methyl silane environment-friendly asphalt separant is characterized in that: the feed comprises the following raw materials in parts by weight: 3-5 parts of methyl silane, 8-10 parts of kelp extract, 0.2-0.5 part of polyethylene glycol 20000, 4-6 parts of peregal, 1-3 parts of sodium aminotriacetate, 0.1-0.3 part of gelatin and 0.2-0.5 part of anti-aging agent;
the asphalt separant is prepared by the following steps:
step S1: adding methylsilane, herba Zosterae Marinae extract and polyethylene glycol 20000 into a stirring kettle, stirring at rotation speed of 300-500r/min and temperature of 60-70 deg.C for 10-15min to obtain a mixture;
step S2: adding peregal, sodium aminotriacetate and gelatin into a stirring kettle, stirring for 15-20min at the rotation speed of 200-800 r/min, adding the mixture and an anti-aging agent, stirring for 1-1.5h at the rotation speed of 500-800r/min, and adjusting the pH value to 6.5-7.5 to obtain the asphalt separant.
2. The water-soluble methyl silane environment-friendly asphalt separant according to claim 1, wherein: the anti-aging agent is prepared by the following steps:
step A1: adding a sulfuric acid solution and deionized water into a reaction kettle, stirring and adding o-nitroaniline at the rotation speed of 150 plus 200r/min and the temperature of 3-5 ℃, dropwise adding a sodium nitrate solution for 0.5-0.8h after stirring for 10-15min, continuously stirring for 1-1.5h after dropwise adding is finished, adding p-methylphenol, continuously stirring for 3-5min, adjusting the pH value of the reaction solution to 7-9, continuously stirring for 2-3h, adding ethanol, a sodium hydroxide solution and a glucose solution, reacting for 1-1.5h at the temperature of 40-50 ℃, adding zinc powder, continuously reacting for 0.5-0.8h at the temperature of 85-90 ℃ to prepare an intermediate 1, and mixing the intermediate 1, nitrogen-succinimide, benzoyl peroxide bromide, bromine, and glucose to obtain an intermediate 1, Adding carbon tetrachloride into a reaction kettle, reacting for 8-10h at the temperature of 80-90 ℃ to obtain an intermediate 2, adding the intermediate 2, a potassium carbonate solution and tetraethylammonium bromide into the reaction kettle, and performing reflux reaction for 1-1.5h at the temperature of 120-130 ℃ to obtain an intermediate 3;
step A2: adding diphenylamine, deionized water and concentrated hydrochloric acid into a reaction kettle, adding acetic anhydride and a sodium acetate solution under the conditions of a rotation speed of 200-;
step A3: adding the intermediate 6, ethanol and concentrated sulfuric acid into a reaction kettle, performing reflux reaction at the rotation speed of 150-, adjusting the pH value of the reaction solution to 8, adding glacial acetic acid, and uniformly mixing to obtain an intermediate 10;
step A4: dissolving cyanuric chloride in acetone, adding an intermediate 10, reacting for 5-6h at the rotation speed of 200-50 ℃ at 300r/min to obtain an intermediate 11, adding the intermediate 11, chlorobenzene and aluminum trichloride into a reaction kettle, stirring and adding magnesium powder at the rotation speed of 150-200r/min and the temperature of 3-5 ℃, stirring for 15-30min, adding toluene at the temperature of 0-3 ℃, stirring for 1-2h, continuously stirring for 10-15h at the temperature of 20-25 ℃, adding resorcinol, and reacting for 4-6h at the temperature of 80-90 ℃ to obtain an intermediate 12;
step A5: adding the intermediate 12, 3-bromopropylene, sodium bicarbonate and acetone into a reaction kettle, performing reflux reaction for 6-8h at the temperature of 60-65 ℃ to obtain an intermediate 13, adding the intermediate 13, styrene and tetrahydrofuran into the reaction kettle, adding azobisisobutyronitrile at the rotation speed of 200-300r/min at the temperature of 70-80 ℃ to react for 3-4h, and precipitating with petroleum ether to obtain the anti-aging agent.
3. The water-soluble methyl silane environment-friendly asphalt separant according to claim 2, wherein: the mass ratio of the sulfuric acid solution, the o-nitroaniline, the sodium nitrate solution, the p-methylphenol, the ethanol, the sodium hydroxide solution, the glucose solution and the zinc powder in the step A1 is 13.5g to 30.6g to 6.48g to 10mL to 10g to 15g to 1.3g, the mass fraction of the sulfuric acid solution is 98%, the mass fraction of the sodium nitrate solution is 30%, the mass fraction of the sodium hydroxide solution is 20%, the mass fraction of the glucose solution is 28.5%, the mass ratio of the intermediate 1, the nitrogen-bromosuccinimide, the benzoyl peroxide and the carbon tetrachloride is 0.15mol to 0.3g to 200mL, the mass ratio of the intermediate 2, the potassium carbonate solution and the tetraethylammonium bromide is 5g to 80mL to 2mL, and the mass fraction of the potassium carbonate solution is 12%.
4. The water-soluble methyl silane environment-friendly asphalt separant according to claim 2, wherein: the dosage ratio of the diphenylamine, the deionized water, the concentrated hydrochloric acid, the acetic anhydride and the sodium acetate solution in the step A2 is 3.5g:90mL:4mL:6mL:12mL, the mass fraction of the concentrated hydrochloric acid is 25%, the dosage molar ratio of the intermediate 4 to the liquid-state methane chloride is 1:2, the dosage of the aluminum trichloride is 5-8% of the mass of the intermediate 4, the dosage ratio of the intermediate 5, the magnesium sulfate, the deionized water and the potassium permanganate solution is 3.5g:10g:175mL:50mL, and the mass fraction of the potassium permanganate solution is 23%.
5. The water-soluble methyl silane environment-friendly asphalt separant according to claim 2, wherein: the molar ratio of the intermediate 6 to the ethanol in the step A3 is 1:1, the dosage of concentrated sulfuric acid is 20% of the mass of the intermediate 6, the mass fraction of the concentrated sulfuric acid is 95%, the dosage ratio of the intermediate 7, the intermediate 3, dibutyltin oxide and o-dichlorobenzene is 0.01mol:0.01mol:0.1g:6mL, the dosage ratio of the intermediate 8, sulfur and iodine is 125mmol:250mmol:0.47mmol, the dosage ratio of the intermediate 9 to the hydrochloric acid solution is 1g:5mL, the mass fraction of the hydrochloric acid solution is 18%, and the dosage of glacial acetic acid is 3% of the total volume of the reaction solution.
6. The water-soluble methyl silane environment-friendly asphalt separant according to claim 2, wherein: the molar ratio of the cyanuric chloride to the intermediate 10 in the step A4 is 1:1, and the molar ratio of the intermediate 11, chlorobenzene, aluminum trichloride, magnesium powder, toluene and resorcinol is 0.1mol:100mL:0.25mol:1g:20g:0.13 mol.
7. The water-soluble methyl silane environment-friendly asphalt separant according to claim 2, wherein: the molar ratio of the intermediate 12, the 3-bromopropylene and the sodium bicarbonate in the step A5 is 1:1:1, the molar ratio of the intermediate 13 to the styrene is 1:71, and the dosage of the azobisisobutyronitrile is 1-1.2% of the mass sum of the intermediate 13 and the styrene.
CN202110042104.9A 2021-01-13 2021-01-13 Water-soluble methyl silane environment-friendly asphalt separant Withdrawn CN112852018A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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CN113502062A (en) * 2021-07-19 2021-10-15 安徽省奥佳建材有限公司 Antioxidant composite waterproof coiled material
CN116425496A (en) * 2023-03-17 2023-07-14 泰山石膏（江阴）有限公司 High-strength gypsum-based fiber board and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113502062A (en) * 2021-07-19 2021-10-15 安徽省奥佳建材有限公司 Antioxidant composite waterproof coiled material
CN116425496A (en) * 2023-03-17 2023-07-14 泰山石膏（江阴）有限公司 High-strength gypsum-based fiber board and preparation method thereof
CN116425496B (en) * 2023-03-17 2024-04-19 泰山石膏（江阴）有限公司 High-strength gypsum-based fiber board and preparation method thereof

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Application publication date: 20210528