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CN113214159A - Preparation method of asphalt emulsifier - Google Patents

Preparation method of asphalt emulsifier Download PDF

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Publication number
CN113214159A
CN113214159A CN202110666538.6A CN202110666538A CN113214159A CN 113214159 A CN113214159 A CN 113214159A CN 202110666538 A CN202110666538 A CN 202110666538A CN 113214159 A CN113214159 A CN 113214159A
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acid
emulsifier
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邹亚丽
阳习春
刘小林
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Hunan Linte Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
    • C07D233/04—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
    • C07D233/20—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with substituted hydrocarbon radicals, directly attached to ring carbon atoms
    • C07D233/24—Radicals substituted by nitrogen atoms not forming part of a nitro radical
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2395/00—Bituminous materials, e.g. asphalt, tar or pitch

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Abstract

The invention discloses a preparation method of an asphalt emulsifier, which comprises the following steps: s1, synthesizing an intermediate: adding fatty acid, aminobenzoic acid and a first catalyst into a first reactor under an inert atmosphere, heating to a preset temperature for reaction under a vacuum environment, cooling when the acid value is lower than a set value, and then sequentially performing alkali washing, filtering and drying treatment to obtain an intermediate; s2, synthesizing an emulsifier: and (4) adding the intermediate obtained in the step (S1) into a second reactor, adding polyamine and a second catalyst into the second reactor in an inert atmosphere, reacting for a set time at different temperatures, ending the reaction after the acid value reaches a target value, removing unreacted polyamine, then cooling, adding water, adding acrylic acid for reaction, and adjusting the pH value after the temperature reaches the set temperature to obtain the emulsifier. The synthetic emulsifier and the emulsifier sold in the market emulsify the asphalt, and the result shows that the emulsifier has obvious comprehensive performance advantage.

Description

Preparation method of asphalt emulsifier
Technical Field
The invention belongs to the technical field of emulsified asphalt, and particularly relates to a preparation method of an asphalt emulsifier.
Background
The emulsified asphalt technology is one of the main means of road maintenance at present, and the adoption of emulsified asphalt for paving a road surface has the advantages of energy conservation, construction season prolongation, pollution reduction and the like. The traditional emulsified asphalt refers to cationic emulsified asphalt for roads, which is mainly an emulsified system of quaternary ammonium salt containing chloride ions. Meanwhile, the emulsified asphalt is used as an inert thermoplastic product, has excellent waterproof and anticorrosion performances, and has the self-repairing performance of typical thermoplastic resin. Unfortunately, there has been a long-felt lack of systematic research and development based on high performance emulsified asphalt products for corrosion and water protection.
In the process of changing asphalt into emulsified asphalt, an emulsifier needs to be introduced, and a conventional cationic emulsifier contains chloride ions. In recent years, with the continuous progress of the synthesis and emulsification technology of polymer emulsion, novel water-based waterproof and anticorrosive coatings are rapidly developed, and the water-based, environment-friendly and sustainable coating is a great trend in the development of the coating industry. The waterproof and anticorrosive emulsified asphalt is a smooth and crude product with high performance and low cost, and develops the high-quality application market of the emulsified asphalt. However, the coating for corrosion prevention and water prevention is mainly a negative nonionic system, and the coating related to emulsified asphalt needs to be modified by adding other types of polymers, such as epoxy emulsion, styrene-butadiene emulsion, acrylic emulsion and the like (the water-based polymers in the coating field are all negative nonionic systems). The cationic emulsifier in the present stage has narrow emulsification range and poor compatibility, and the problem of emulsifier migration is easy to occur in an emulsification system, and the prepared emulsified asphalt is difficult to reach the relevant standards of the emulsion for anticorrosive and waterproof coatings, such as mechanical stability, low-temperature stability, metal ion stability, freeze-thaw stability, water absorption, salt spray resistance and the like. It can be said that the development level of asphalt emulsifier, which is the core of the whole technology, affects the development and application of emulsified asphalt products.
Chinese patent CN201911395423.7 discloses an emulsifier for cold recycling and a preparation method thereof, which synthesizes a cationic asphalt emulsifier with a brand-new structure based on redesign of molecular structure, and fully exerts the synergistic effect of compounding, so that the prepared emulsifier can simultaneously give consideration to the cost and performance effects. However, the cationic asphalt emulsifier has the disadvantages of narrow emulsification range, poor compatibility with coating products and complex preparation method.
At present, the emulsified asphalt technology in China has a great gap compared with the developed western countries, and the most main problems are that the performance and the stability of an emulsifier are not enough, the emulsifying effect is improved only by relying on a large amount of emulsifier complex formulation exploration experiments, the emulsified asphalt with good particle size cannot be formed, and the stability of the performance of the emulsified asphalt product cannot be ensured.
Therefore, it is highly desirable to develop a non-ionic asphalt emulsifier, which has good compatibility with conventional water-based polymers, low emulsifier usage and no migration, and the prepared emulsified asphalt can meet the standards of emulsions for anticorrosive and waterproof coatings.
Disclosure of Invention
Aiming at the problems that the emulsification range of an emulsification system is narrow, the compatibility is poor, the emulsifier is easy to migrate, and the prepared emulsified asphalt is difficult to reach the relevant standards of the emulsion for anticorrosive and waterproof coatings in the prior art, the invention aims to provide a preparation method of an asphalt emulsifier.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a preparation method of an asphalt emulsifier, which comprises the following steps:
s1. synthesis of intermediates: adding fatty acid, aminobenzoic acid and a first catalyst into a first reactor under an inert atmosphere, heating to a preset temperature for reaction under a vacuum environment, cooling when the acid value is lower than a set value, and then sequentially performing alkali washing, filtering and drying treatment to obtain an intermediate;
s2 synthetic emulsifier: and (4) adding the intermediate obtained in the step (S1) into a second reactor, adding polyamine and a second catalyst into the second reactor in an inert atmosphere, reacting for a set time at different temperatures, ending the reaction after the acid value reaches a target value, removing unreacted polyamine, then cooling, adding water, adding acrylic acid for reaction, and adjusting the pH value after the temperature reaches the set temperature to obtain the emulsifier.
In the step S1, the fatty acid is unsaturated fatty acid or saturated fatty acid, the number of carbon atoms in a carbon chain is 5-20, the value of n represents the number of aminocarboxylic acids, and the structural formula is shown as formula I.
Figure 578213DEST_PATH_IMAGE001
Formula I
In a preferred embodiment, the fatty acid is one or more of lauric acid, soya oil acid, eleostearic acid, tall oil acid, linoleic acid, linolenic acid, arachidonic acid, and naphthenic acid.
More preferably, lauric acid or naphthenic acid is used as the fatty acid.
In step S1, the aminobenzoic acid has three isomers, and is any one of anthranilic acid, m-aminobenzoic acid, and p-aminobenzoic acid, and the mass ratio of the fatty acid to the aminobenzoic acid is 1.05-1.5: 1.
In a preferred scheme, p-aminobenzoic acid is adopted as the aminobenzoic acid, and the aminobenzoic acid is fatty acid: adding para aminobenzoic acid = 1.1-1.2: 1.
In step S1, the first catalyst is one or a combination of triethylamine, triethanolamine, tetrabutylammonium bromide, 2,4, 6-tris (dimethylaminomethyl) phenol, and organotin; the addition amount is 0.01wt% to 0.05wt% of the total reactants.
In a preferred embodiment, tetrabutylammonium bromide and 2,4, 6-tris (dimethylaminomethyl) phenol are used as the first catalyst.
In step S1, the reaction temperature of the fatty acid, the aminobenzoic acid and the first catalyst is 110-130 ℃.
In a preferred embodiment, the reaction temperature of the fatty acid, the aminobenzoic acid and the first catalyst is 120 ℃.
In step S2, the polyamine is one or a combination of two or more of diethylenetriamine, triethylenetetramine and tetraethylenepentamine, and an imidazole ring structure is formed by a dehydration reaction of a carboxyl group in the polyamine and an amino group; the intermediate obtained according to the mass ratio of S1: polyamine = 1: 1.1 to 1.3.
In step S2, the second catalyst is one or a combination of more of alumina, boric acid, triphenylphosphine, tetrabutylammonium bromide and organotin, and is used to promote the synthesis of the imidazole ring structure; the addition amount is 0.01wt% to 0.05wt% of the total reactants.
In step S2, the amount of acrylic acid added is determined by the type of polyamine selected and the number of acrylic acids to be incorporated is determined by the desired emulsification effect.
In step S2, the specific process of synthesizing the emulsifier is as follows:
reacting the intermediate, the polyamine and the second catalyst at different temperatures in stages, wherein the reaction is carried out at 120 ℃ for 0.5-2 h, at 130 ℃ for 0.5-2 h, at 140 ℃ for 0.5-2 h, at 150 ℃ for 0.5-2 h, at 160 ℃ for 0.5-2 h, at 170 ℃ for 0.5-2 h, at 180 ℃ for 0.5-2 h, at 190 ℃ for 0.5-2 h, at 200 ℃ for 0.5-2 h and at 220 ℃ for 0.5-2 h, after the acid value reaches a target value, the reaction is finished, vacuumizing at 220 ℃ to remove unreacted amine, cooling to 80 ℃, adding a set amount of water, keeping the temperature to 80 ℃, dropwise adding acrylic acid in proportion, reacting for 1-4 h, adjusting the pH value to 9.5 by using sodium hydroxide, and discharging to obtain the emulsifier.
The imidazole compound has medicinal activity, physiological activity and good surface activity effect, and has very important functions in medicine, life science, industrial products and daily life. The imidazole derivative can have very excellent emulsifying performance when used as a surfactant, and has very important practical effect on systematic research on the synthesis of imidazole surfactants.
The invention synthesizes an imidazole asphalt emulsifier with benzene rings, firstly, fatty acid and aminobenzoic acid are subjected to amidation reaction to prepare a benzoic acid intermediate of a fatty chain, and then intermediate carboxyl is subjected to reaction with a polyamine substance to prepare an anion asphalt emulsifier with an imidazole structure, wherein the prepared emulsified asphalt meets the related national industrial standard of water-based emulsion in the field of refined coating. According to the invention, aminobenzoic acid is introduced into a benzene ring structure to form an imidazoline structure with a benzene ring, so that the emulsifying effect of the emulsifier is greatly improved.
The anionic emulsifier synthesized by the invention has excellent chelation property on metal and concrete base materials, realizes emulsification on the base material petroleum asphalt, and prepares the high-performance waterproof and anticorrosive emulsified asphalt. The emulsified asphalt series has excellent water resistance and corrosion resistance, can be made into high-performance waterproof coatings, anticorrosive coatings and waterproof anticorrosive coatings by adding different fillers and auxiliaries, can be applied to container water-based asphalt underframe paint on a large scale, and can be applied to domestic waterproof engineering on a large scale.
According to the invention, the emulsifier which has a chelation reaction on metal and concrete is synthesized, so that the problem of emulsifier migration which is easy to occur in an external emulsifying system is avoided, meanwhile, the emulsifier adopts a structure without chloride ions, so that the prepared emulsified asphalt has excellent corrosion resistance and waterproof performance, a related application formula system is established, and a proper polymer modified emulsified asphalt is introduced to apply the product to projects such as metal corrosion resistance, building, bridge waterproofing and the like in a large scale.
The preparation method of the emulsifier for asphalt does not use organic solvent in the reaction process, and is a pollution-free pure green production process.
Drawings
FIG. 1 is a chemical reaction equation for preparing a bitumen emulsifier in example 1.
FIG. 2 is a chemical reaction equation for preparing a bitumen emulsifier in example 2.
FIG. 3 is a chemical reaction equation for preparing a bitumen emulsifier in example 3.
Detailed Description
The technical solution of the present invention is explained in detail by the following embodiments and the accompanying drawings.
The invention provides a preparation method of an asphalt emulsifier, which comprises the following steps:
s1. synthesis of intermediates: adding fatty acid, aminobenzoic acid and a first catalyst into a first reactor under an inert atmosphere, heating to a preset temperature for reaction under a vacuum environment, cooling when the acid value is lower than a set value, and then sequentially performing alkali washing, filtering and drying treatment to obtain an intermediate;
s2 synthetic emulsifier: and (4) adding the intermediate obtained in the step (S1) into a second reactor, adding polyamine and a second catalyst into the second reactor in an inert atmosphere, reacting for a set time at different temperatures, ending the reaction after the acid value reaches a target value, removing unreacted polyamine, then cooling, adding water, adding acrylic acid for reaction, and adjusting the pH value after the temperature reaches the set temperature to obtain the emulsifier.
In the step S1, the fatty acid is unsaturated fatty acid or saturated fatty acid, the number of carbon atoms in a carbon chain is 5-20, the value of n represents the number of aminocarboxylic acids, and the structural formula is shown as formula I.
Figure 26512DEST_PATH_IMAGE002
Formula I
The fatty acid is one or more of lauric acid, soya oil acid, eleostearic acid, tall oil acid, linoleic acid, linolenic acid, arachidonic acid and naphthenic acid.
In step S1, the aminobenzoic acid has three isomers, and is any one of anthranilic acid, m-aminobenzoic acid, and p-aminobenzoic acid, and the mass ratio of the fatty acid to the aminobenzoic acid is 1.05-1.5: 1.
In step S1, the first catalyst is one or a combination of triethylamine, triethanolamine, tetrabutylammonium bromide, 2,4, 6-tris (dimethylaminomethyl) phenol, and organotin; the addition amount is 0.01wt% to 0.05wt% of the total reactants.
In step S1, the reaction temperature of the fatty acid, the aminobenzoic acid and the first catalyst is 110-130 ℃.
In step S2, the polyamine is one or a combination of two or more of diethylenetriamine, triethylenetetramine and tetraethylenepentamine, and an imidazole ring structure is formed by a dehydration reaction of a carboxyl group in the polyamine and an amino group; the intermediate obtained according to the mass ratio of S1: polyamine = 1: 1.1 to 1.3.
In step S2, the second catalyst is one or a combination of more of alumina, boric acid, triphenylphosphine, tetrabutylammonium bromide and organotin, and is used to promote the synthesis of the imidazole ring structure; the addition amount is 0.01wt% to 0.05wt% of the total reactants.
In step S2, the amount of acrylic acid added is determined by the type of polyamine selected and the number of acrylic acids to be incorporated is determined by the desired emulsification effect.
In step S2, the specific process of synthesizing the emulsifier is as follows:
reacting the intermediate, the polyamine and the second catalyst at different temperatures in stages, wherein the reaction is carried out at 120 ℃ for 0.5-2 h, at 130 ℃ for 0.5-2 h, at 140 ℃ for 0.5-2 h, at 150 ℃ for 0.5-2 h, at 160 ℃ for 0.5-2 h, at 170 ℃ for 0.5-2 h, at 180 ℃ for 0.5-2 h, at 190 ℃ for 0.5-2 h, at 200 ℃ for 0.5-2 h and at 220 ℃ for 0.5-2 h, after the acid value reaches a target value, the reaction is finished, vacuumizing at 220 ℃ to remove unreacted amine, cooling to 80 ℃, adding a set amount of water, keeping the temperature to 80 ℃, dropwise adding acrylic acid in proportion, reacting for 1-4 h, adjusting the pH value to 9.5 by using sodium hydroxide, and discharging to obtain the emulsifier.
The invention has the difficulties that the asphalt still has high-efficiency waterproof and anticorrosive performance after being hydrated, the traditional mode of heating or adding solvent is changed, the prepared emulsifier is not easy to migrate, the excellent anticorrosive and salt mist resistant capability of the original asphalt is not influenced, and the prepared emulsified asphalt needs to have excellent stability and excellent compatibility with other high molecular polymer emulsions on the market.
The asphalt emulsifier disclosed by the invention has the advantages that the asphalt has an ultra-small particle size after being subjected to water-based emulsification, has good compatibility with more emulsions on the market, and is good in mechanical stability, excellent in calcium ion stability and longer in storage stability. The prepared waterproof coating has good water resistance, high-temperature creep self-healing performance and long-term water resistance; the obtained anticorrosive coating has excellent adhesion to a base material, a paint film has high-efficiency barrier property, and the corrosion of external acid-base salt to the base material can be effectively prevented. The application requirements in the relevant fields of metal corrosion prevention, building waterproofing, adhesives and the like are met.
In this example, unless otherwise specified, all reagents used were common commercial products or prepared by conventional means, and the equipment used was conventional in the art, and the following are some examples of the inventors in the experiment:
example 1
A preparation method of an asphalt emulsifier comprises the following steps:
(1) under the protection of nitrogen atmosphere, adding 220kg of lauric acid, 137kg of anthranilic acid and tetrabutylammonium bromide (the addition amount is 0.02wt% of the total reactants) into a reaction kettle, heating to 120 ℃, vacuumizing for reaction, cooling when the amine value is =0 mg KOH/g, performing alkali washing, filtering, and drying to obtain an intermediate;
(2) adding the intermediate into a reaction kettle, charging nitrogen to discharge oxygen, adding 115kg of diethylenetriamine and aluminum oxide (the addition amount is 0.01wt% of the total reactants), carrying out temperature rise reaction in stages, heating to 120 ℃ for 1h, 130 ℃ for 1h, 140 ℃ for 1h, 150 ℃ for 1h, 160 ℃ for 1h, 170 ℃ for 1h, 180 ℃ for 1h, 190 ℃ for 1h, 200 ℃ for 1h, and 220 ℃ for 1h, wherein the acid value =0 mg KOH/g, finishing the reaction, vacuumizing at 220 ℃ to remove unreacted amine, cooling to 80 ℃, adding 300kg of water, slowly dropwise adding 50kg of acrylic acid, carrying out constant temperature reaction for 2h, adding a sodium hydroxide solution to adjust the pH value to 9.5, and discharging to obtain the emulsifier.
Example 2
A preparation method of an asphalt emulsifier comprises the following steps:
(1) under the protection of nitrogen atmosphere, adding 282kg of oleic acid, 137kg of m-aminobenzoic acid and 2,4, 6-tris (dimethylaminomethyl) phenol (the addition amount is 0.02wt% of the total reactants) into a reaction kettle, heating to 120 ℃, vacuumizing for reaction, cooling when the amine value is =0 mg KOH/g, carrying out alkali washing, filtering and drying to obtain an intermediate;
(2) adding the intermediate into a reaction kettle, filling nitrogen to discharge oxygen, adding 115kg of diethylenetriamine and boric acid (the addition amount is 0.01wt% of the total reactants), and carrying out temperature rise reaction in stages, wherein the temperature is 120 ℃ for 1h, the temperature is 130 ℃ for 1h, the temperature is 140 ℃ for 1h, the temperature is 150 ℃ for 1h, the temperature is 160 ℃ for 1h, the temperature is 170 ℃ for 1h, the temperature is 180 ℃ for 1h, the temperature is 190 ℃ for 1h, the temperature is 200 ℃ for 1h, and the temperature is 220 ℃ for 1 h. And (3) finishing the reaction with the acid value =0 mg KOH/g, vacuumizing at 220 ℃ to remove unreacted amine, cooling to 80 ℃, adding 300kg of water, slowly dropwise adding 50kg of acrylic acid, reacting at constant temperature for 2 hours, adding a sodium hydroxide solution to adjust the pH value to 9.5, and discharging to obtain the emulsifier.
Example 3
A preparation method of an asphalt emulsifier comprises the following steps:
(1) under the protection of nitrogen atmosphere, adding 126kg of naphthenic acid, 137kg of p-aminobenzoic acid and tetrabutylammonium bromide (the addition amount is 0.02wt% of the total reactants) into a reaction kettle, heating to 120 ℃, vacuumizing for reaction, cooling when the amine value is =0 mg KOH/g, performing alkaline washing, filtering, and drying to obtain an intermediate;
(2) adding the intermediate into a reaction kettle, charging nitrogen to discharge oxygen, adding 115kg of diethylenetriamine and triphenylphosphine (the addition amount is 0.01wt% of the total reactants), carrying out temperature rise reaction in stages, heating to 120 ℃ for 1h, 130 ℃ for 1h, 140 ℃ for 1h, 150 ℃ for 1h, 160 ℃ for 1h, 170 ℃ for 1h, 180 ℃ for 1h, 190 ℃ for 1h, 200 ℃ for 1h, and 220 ℃ for 1h, wherein the acid value =0 mg KOH/g, finishing the reaction, vacuumizing to remove unreacted amine at 220 ℃, cooling to 80 ℃, adding 300kg of water, slowly adding 50kg of acrylic acid dropwise, carrying out constant temperature reaction for 2h, adding a sodium hydroxide solution to adjust the pH value to 9.5, and discharging to obtain the emulsifier.
Application examples 1 to 3
The emulsifying agent (model LT-4003) prepared in the embodiments 1, 2 and 3 of the invention is used for emulsifying asphalt, the emulsified asphalt is respectively the application examples 1, 2 and 3, and the asphalt emulsifying process and the process are as follows:
dissolving the emulsifier and stabilizer (hydroxyethyl cellulose ether) in water to obtain soap liquid, and heating to 65 deg.C; heating the asphalt to 130 ℃, simultaneously adding the soap solution and the asphalt into a colloid mill, and shearing and dispersing at a high speed for 1min to obtain the emulsified asphalt.
Comparative example
Dissolving commercially available non-imidazoline emulsifier (cetyl quaternary ammonium salt) and stabilizer in water to obtain soap solution, and heating to 65 deg.C; heating the asphalt to 130 ℃, simultaneously adding the soap solution and the asphalt into a colloid mill, and shearing and dispersing at a high speed for 1min to obtain the emulsified asphalt.
Test results
Table 1 comparison of Performance test results of application examples 1 to 3 and comparative examples
Test items Experimental methods Technical requirements Application example 1 Application example 2 Application example 3 Comparative example
Penetration/0.1 mm T0606 40~120 78 81 85 90
5 ℃ ductility/cm T0605 ≥20 46 50 56 21
Softening point/. degree.C T0604 ≥50 76 79 80 51
Solubility/%) T0607 ≥97.5 99.8 99.7 99.9 98
Storage stability/5 d T0655 2.6 0.4 0.8 0.1 2.0
The results of tests conducted by referring to the JTG-F40 method of the department of transportation in Table 1 are superior to those of the comparative examples in the test results of application examples 1-3, and particularly in the aspects of low-temperature ductility and storage stability, the application example 3 has the optimal comprehensive performance, which shows that the imidazoline structure has a very good effect on asphalt emulsification, and imidazoline prepared from naphthenic acid has the optimal comprehensive effect.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. The preparation method of the asphalt emulsifier is characterized by comprising the following steps:
s1. synthesis of intermediates: adding fatty acid, aminobenzoic acid and a first catalyst into a first reactor under an inert atmosphere, heating to a preset temperature for reaction under a vacuum environment, cooling when the acid value is lower than a set value, and then sequentially performing alkali washing, filtering and drying treatment to obtain an intermediate;
s2 synthetic emulsifier: and (4) adding the intermediate obtained in the step (S1) into a second reactor, adding polyamine and a second catalyst into the second reactor in an inert atmosphere, reacting for a set time at different temperatures, ending the reaction after the acid value reaches a target value, removing unreacted polyamine, then cooling, adding water, adding acrylic acid for reaction, and adjusting the pH value after the temperature reaches the set temperature to obtain the emulsifier.
2. The method for preparing the asphalt emulsifier according to claim 1, wherein in step S1, the fatty acid is one or more selected from lauric acid, soya oil acid, eleostearic acid, tall oil acid, linoleic acid, linolenic acid, arachidonic acid, and naphthenic acid.
3. The method for preparing an asphalt emulsifier according to claim 1, wherein in step S1, the aminobenzoic acid is any one of anthranilic acid, m-aminobenzoic acid and p-aminobenzoic acid, and the mass ratio of the fatty acid to the aminobenzoic acid is 1.05-1.5: 1.
4. The preparation method of the asphalt emulsifier according to claim 3, wherein the aminobenzoic acid is p-aminobenzoic acid, and the mass ratio of the fatty acid to the p-aminobenzoic acid is 1.1-1.2: 1.
5. The method for preparing asphalt emulsifier according to claim 1, wherein in step S1, the first catalyst is one or more selected from triethylamine, triethanolamine, tetrabutylammonium bromide, 2,4, 6-tris (dimethylaminomethyl) phenol, and organotin, and the amount of the first catalyst is 0.01wt% to 0.05wt% of the total reactants.
6. The method for preparing the asphalt emulsifier according to claim 1, wherein the reaction temperature of the fatty acid, the aminobenzoic acid and the first catalyst in step S1 is 110-130 ℃.
7. The method for preparing asphalt emulsifier according to claim 6, wherein the reaction temperature of the fatty acid, the aminobenzoic acid and the first catalyst is 120 ℃.
8. The method for preparing asphalt emulsifier according to claim 1, wherein in step S2, the polyamine is one or more selected from diethylenetriamine, triethylenetetramine and tetraethylenepentamine, and the ratio of the intermediate to the polyamine is 1: 1.1 to 1.3.
9. The method for preparing the asphalt emulsifier according to claim 1, wherein in step S2, the second catalyst is one or more of alumina, boric acid, triphenylphosphine, tetrabutylammonium bromide and organotin, and the amount of the second catalyst is 0.01wt% to 0.05wt% of the total reactants.
10. The method for preparing asphalt emulsifier according to claim 1, wherein in step S2, the specific process of synthesizing the emulsifier is as follows:
reacting the intermediate, the polyamine and the second catalyst at different temperatures in stages, wherein the reaction is carried out at 120 ℃ for 0.5-2 h, at 130 ℃ for 0.5-2 h, at 140 ℃ for 0.5-2 h, at 150 ℃ for 0.5-2 h, at 160 ℃ for 0.5-2 h, at 170 ℃ for 0.5-2 h, at 180 ℃ for 0.5-2 h, at 190 ℃ for 0.5-2 h, at 200 ℃ for 0.5-2 h and at 220 ℃ for 0.5-2 h, after the acid value reaches a target value, the reaction is finished, vacuumizing at 220 ℃ to remove unreacted amine, cooling to 80 ℃, adding a set amount of water, keeping the temperature to 80 ℃, dropwise adding acrylic acid in proportion, reacting for 1-4 h, adjusting the pH value to 9.5 by using sodium hydroxide, and discharging to obtain the emulsifier.
CN202110666538.6A 2021-06-16 2021-06-16 Preparation method of asphalt emulsifier Pending CN113214159A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104941509A (en) * 2015-05-11 2015-09-30 中国海洋石油总公司 Micro-surfacing slow cracking and rapid setting asphalt emulsifier and preparation method thereof
CN107739339A (en) * 2017-11-22 2018-02-27 潍坊学院 A kind of difunctional asphalt emulsifier and preparation method thereof
CN109628089A (en) * 2019-01-18 2019-04-16 山东建筑大学 A kind of pitch-based graphene-based pitch emulsifier and preparation method thereof
CN113307986A (en) * 2021-06-15 2021-08-27 湖南林特新材料科技有限责任公司 Anticorrosive waterproof emulsified asphalt and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104941509A (en) * 2015-05-11 2015-09-30 中国海洋石油总公司 Micro-surfacing slow cracking and rapid setting asphalt emulsifier and preparation method thereof
CN107739339A (en) * 2017-11-22 2018-02-27 潍坊学院 A kind of difunctional asphalt emulsifier and preparation method thereof
CN109628089A (en) * 2019-01-18 2019-04-16 山东建筑大学 A kind of pitch-based graphene-based pitch emulsifier and preparation method thereof
CN113307986A (en) * 2021-06-15 2021-08-27 湖南林特新材料科技有限责任公司 Anticorrosive waterproof emulsified asphalt and preparation method thereof

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