CN113698596B - Cationic asphalt emulsifier, preparation method thereof and asphalt emulsion preparation method - Google Patents
Cationic asphalt emulsifier, preparation method thereof and asphalt emulsion preparation method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/48—Polymers modified by chemical after-treatment
- C08G69/50—Polymers modified by chemical after-treatment with aldehydes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/34—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids using polymerised unsaturated fatty acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/48—Polymers modified by chemical after-treatment
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- 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
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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/30—Adapting or protecting infrastructure or their operation in transportation, e.g. on roads, waterways or railways
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- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention discloses a cationic asphalt emulsifier, a preparation method thereof and a method for preparing asphalt emulsion by adopting the cationic asphalt emulsifier. The cationic asphalt emulsifier is prepared from dimer acid, polyamine, cationic etherifying agent CHPTAC and paraformaldehyde serving as raw materials according to the weight components of the corresponding components. The cationic asphalt emulsifier is prepared through amidation reaction and quaternization reaction, and the network structure of the asphalt emulsifier is increased through adding paraformaldehyde to strengthen the adhesion strength of asphalt and stone. The asphalt emulsifier provided by the invention has excellent emulsifying property for different types of asphalt, can be widely compatible with various aggregates, has good coating property, and can be suitable for micro-surfacing construction of high-activity stones and high-temperature weather.
Description
Technical Field
The invention relates to the technical field of asphalt emulsifiers, in particular to a cationic asphalt emulsifier, a preparation method of the asphalt emulsifier and a method for preparing asphalt emulsion by adopting the cationic asphalt emulsifier.
Background
Asphalt emulsifiers are one type of surfactant. The chemical structure of the polymer consists of lipophilic groups and hydrophilic groups. The surfactant can be adsorbed at the interface between asphalt particles and water, so that the free energy of the interface between asphalt and water is obviously reduced, and the surfactant forms a uniform and stable emulsion. Asphalt emulsifiers can be classified into quick-cracking type, medium-cracking type and slow-cracking type according to their demulsification speed, wherein the slow-cracking type is also classified into slow-cracking quick-setting type and slow-cracking slow-setting type according to different construction processes.
At present, most of slow-cracking quick-setting asphalt emulsifiers in the market are amide polyamines, most of the lipophilic ends are long-chain fatty acids or modified fatty acids, and the hydrophilic ends are polyamines.
Disclosure of Invention
The invention aims at overcoming the technical defects in the prior art, and provides a cationic asphalt emulsifier, a preparation method of the asphalt emulsifier and a preparation method of asphalt emulsion.
The technical scheme adopted for realizing the purpose of the invention is as follows:
the cationic asphalt emulsifier consists of the following components in parts by weight:
20-30 parts of dimer acid, 5-20 parts of polyamine, 5-25 parts of cationic etherifying agent CHPTAC and 3-10 parts of paraformaldehyde.
Wherein, the dimer acid is dimer fatty acid, the molecular weight of the dimer acid is large, and simultaneously, the dimer acid has two-COOH functional groups, and the mixing effect of the emulsifier on stones is better.
Specifically, the dimerized fatty acid is selected from one or more of linoleic acid dimer acid, palmitic acid dimer acid and dehydrated castor oil dimer acid.
The polyamine is one or more of triethylene tetramine, tetraethylene pentamine, polyethylene polyamine and aminoethylpiperazine, and the amine can effectively delay the mixing time during application and ensure normal construction.
The cationic etherifying agent is a 3-chloro-2-hydroxypropyl trimethyl ammonium chloride aqueous solution with the solid content of 50% -70%.
A method for preparing a cationic asphalt emulsifier, comprising the following steps:
adding dimer acid into a four-mouth bottle, heating to 80 ℃, slowly adding polyamine into the four-mouth bottle, stirring, heating to 150 ℃ within half an hour, preserving heat for reaction for 6-10 hours, cooling to 60 ℃ until no distillate exists in the reaction, slowly dropwise adding a cationic etherifying agent, controlling the temperature to be not more than 80 ℃, preserving heat for 5 hours at 70-80 ℃ after dropwise adding, cooling to 50-60 ℃, slowly adding paraformaldehyde, controlling the temperature to be not more than 70 ℃, preserving heat for 4 hours at 70-80 ℃ after dropwise adding, cooling to 50-60 ℃ and discharging to obtain the asphalt emulsifier.
The invention also provides a method for preparing asphalt emulsion by using the cationic asphalt emulsifier, which comprises the following steps of preparing the cationic asphalt emulsifier into an aqueous solution, wherein the cationic asphalt emulsifier accounts for 2.0-2.6% of the mass of the asphalt emulsion, adjusting the pH value to 2-3 by using a hydrochloric acid solution, adding the cationic styrene-butadiene latex, the addition amount of which is 3-5% of the asphalt emulsion, and heating to 50-60 ℃; preheating a colloid mill to 50-60 ℃, adding asphalt at 120-140 ℃, and shearing and mixing by the colloid mill to obtain asphalt emulsion.
The cationic asphalt emulsifier of the invention uses dimer acid, which has a molecular weight twice that of common fatty acid, and can be connected with one hydrophilic end, and uses cationic etherifying agent to carry out quaternization reaction, thus delaying mixing and greatly improving the broad spectrum of the product. The addition of paraformaldehyde increases the net structure of the emulsifier, enhances the bonding strength of asphalt and stone, and prolongs the service life of the road.
The cationic asphalt emulsifier provided by the invention has good emulsifying effect for different asphalt. In different construction seasons, the method has good application effect on different stones and environments.
The cationic asphalt emulsifier of the invention has the following advantages in general:
(1) The molecular weight of the emulsifier is doubled by using dimer acid as an oil-philic end, so that the HLB value range of the emulsifier is enlarged, and the emulsifying capacity of the emulsifier for various brands of asphalt, such as middle sea, liaohe, qilu and the like, and the adaptability of the emulsifier to different stones, such as diabase, amphibole, basalt and the like are improved.
(2) The cationic etherifying agent is added to carry out quaternization reaction, so that the emulsifier has partial positive charges, and the negative charges on the surface of stone can be neutralized, thereby achieving the aim of delaying mixing.
(3) By adding paraformaldehyde, the net structure of the emulsifier is enhanced, so that the adhesiveness of asphalt and stone can be increased.
The emulsified asphalt produced by the emulsifier has great advantages on compatibility of various stones, mixing flexibility and later demulsification and strength increasing time.
Detailed Description
Example 1
A method for preparing a cationic asphalt emulsifier, comprising the following steps:
adding 30 parts of linoleic acid dimer acid into a reaction kettle, stirring and heating to 80 ℃, adding 20 parts of polyethylene polyamine into the kettle, stirring and heating to 150 ℃ within half an hour, preserving heat and reacting for 6-10 hours until no distillate exists in the reaction, then cooling to 60 ℃, slowly dropwise adding 5 parts of cationic etherifying agent, controlling the temperature to be not more than 80 ℃, preserving heat for 5 hours at 70-80 ℃, then cooling to 50-60 ℃, slowly adding 10 parts of paraformaldehyde, controlling the temperature to be not more than 70 ℃, preserving heat for 4 hours at 70-80 ℃ after dropwise adding, and then cooling to 50-60 ℃ and discharging to obtain the cationic asphalt emulsifier.
Preparation of emulsified asphalt
10g of the prepared asphalt emulsifier (accounting for 2.0 percent of emulsified asphalt) is taken, water 165 is added, 30 percent hydrochloric acid is used for adjusting the pH value to 2 to 3, 15g of cationic styrene-butadiene latex is added to prepare soap solution, and the soap solution is heated to 60 ℃; 300g of Zhonghai 70# asphalt is taken and heated to 130-140 ℃; the colloid mill was preheated to 60 ℃. And mixing the soap solution with asphalt through a colloid mill to obtain uniform cationic asphalt emulsion.
Asphalt emulsion Performance test, table 1
TABLE 1
According to the grading range recommended in the micro-surfacing and slurry seal technical guidelines in China, an MS-3 grading standard is adopted in the test, and the emulsified asphalt mixture is tested:
| detecting items | Unit (B) | Standard of | Detection result | Test method |
| Mixing time (30 ℃ C.) | s | ≥120 | >120 | ISSA TB 113 |
| Demulsification time | min | -- | 5 | T 0753-1993 |
| The cohesive force test is not less than | N.m | 30min1.2 | 1.4 | T 0754-2011 |
TABLE 2
Example 2
A method for preparing a cationic asphalt emulsifier, comprising the following steps:
adding 20 parts of palmitic acid dimer acid into a reaction kettle, stirring and heating to 80 ℃, adding 10 parts of triethylene tetramine into the kettle, stirring and heating to 150 ℃ within half an hour, preserving heat and reacting for 6-10 hours until no distillate exists in the reaction, then cooling to 60 ℃, slowly dropwise adding 25 parts of cationic etherifying agent, controlling the temperature to be not more than 80 ℃, preserving heat for 5 hours at 70-80 ℃, then cooling to 50-60 ℃, slowly dropwise adding 10 parts of paraformaldehyde, controlling the temperature to be not more than 70 ℃, preserving heat for 4 hours at 70-80 ℃ after dropwise adding, and then cooling to 50-60 ℃ and discharging to obtain the cationic asphalt emulsifier.
Preparation of emulsified asphalt
Taking 11g of the prepared asphalt emulsifier (accounting for 2.2 percent of emulsified asphalt), adding 180g of water, adjusting the pH value to 2-3 by 30 percent hydrochloric acid, adding 15g of cationic styrene-butadiene latex, preparing soap solution, and heating to 60 ℃; 300g of Liaohe 70# asphalt is taken and heated to 130-140 ℃; the colloid mill was preheated to 60 ℃. And mixing the soap solution with asphalt through a colloid mill to obtain uniform cationic asphalt emulsion.
The asphalt emulsion performance test of example 2, see table 3,
TABLE 3 Table 3
According to the grading range recommended in the micro-surfacing and slurry seal technical guidelines in China, the test adopts MS-3 grading standard to test the emulsified asphalt mixture, see Table 4,
| detecting items | Unit (B) | Standard of | Detection result | Test method |
| Mixing time (30 ℃ C.) | s | ≥120 | >120 | ISSA TB 113 |
| Demulsification time | min | -- | 5 | T 0753-1993 |
| The cohesive force test is not less than | N.m | 30min1.2 | 1.4 | T 0754-2011 |
TABLE 4 Table 4
Example 3
A method for preparing a cationic asphalt emulsifier, comprising the following steps:
adding 25 parts of dimer acid into a reaction kettle, stirring and heating to 80 ℃, adding 15 parts of tetraethylenepentamine into the kettle, stirring and heating to 150 ℃ within half an hour, preserving heat and reacting for 6-10 hours until no distillate exists in the reaction, then cooling to 60 ℃, slowly dropwise adding 13 parts of cationic etherifying agent, controlling the temperature to be not more than 80 ℃, preserving heat for 5 hours at 70-80 ℃, then cooling to 50-60 ℃, slowly dropwise adding 6 parts of paraformaldehyde, controlling the temperature to be not more than 70 ℃, preserving heat for 4 hours at 70-80 ℃ after dropwise adding, and then cooling to 50-60 ℃ and discharging to obtain the cationic asphalt emulsifier.
Preparation of emulsified asphalt
The preparation procedure was the same as in example 2 except that asphalt was Qilu70#.
Asphalt emulsion performance tests are shown in table 5.
TABLE 5
According to the grading range recommended in the micro-surfacing and slurry seal technical guidelines in China, an MS-3 grading standard is adopted in the test, and the emulsified asphalt mixture is tested: see Table 6
| Detecting items | Unit (B) | Standard of | Detection result | Test method |
| Mixing time (30 ℃ C.) | s | ≥120 | >120 | ISSA TB 113 |
| Demulsification time | min | -- | 8 | T 0753-1993 |
| The cohesive force test is not less than | N.m | 30min1.2 | 1.4 | T 0754-2011 |
TABLE 6
Example 4
A method for preparing a cationic asphalt emulsifier, comprising the following steps:
adding 25 parts of linoleic acid dimer acid into a reaction kettle, stirring and heating to 80 ℃, adding 14 parts of aminoethylpiperazine into the kettle, stirring and heating to 150 ℃ within half an hour, preserving heat and reacting for 6-10 hours until no distillate exists in the reaction, then cooling to 60 ℃, slowly dropwise adding 10 parts of cationic etherifying agent, controlling the temperature to be not more than 80 ℃, preserving heat for 5 hours at 70-80 ℃, then cooling to 50-60 ℃, slowly dropwise adding 3 parts of paraformaldehyde, controlling the temperature to be not more than 70 ℃, preserving heat for 4 hours at 70-80 ℃ after dropwise adding, and then cooling to 50-60 ℃ and discharging to obtain the cationic asphalt emulsifier.
Preparation of emulsified asphalt
The preparation procedure was the same as in example 2 except that asphalt was used in the middle sea # 70.
Asphalt emulsion performance test: see Table 7
TABLE 7
According to the grading range recommended in the micro-surfacing and slurry seal technical guidelines in China, an MS-3 grading standard is adopted in the test, and the emulsified asphalt mixture is tested: see the table 8 below for a review of the following,
| detecting items | Unit (B) | Standard of | Detection result | Test method |
| Mixing time (30 ℃ C.) | s | ≥120 | >120 | ISSA TB 113 |
| Demulsification time | min | -- | 7 | T 0753-1993 |
| The cohesive force test is not less than | N.m | 30min1.2 | 1.4 | T 0754-2011 |
TABLE 8
Example 5
A method for preparing a cationic asphalt emulsifier, comprising the following steps:
adding 35 parts of linoleic acid dimer acid into a reaction kettle, stirring and heating to 80 ℃, adding 20 parts of triethylene tetramine into the kettle, stirring and heating to 150 ℃ within half an hour, preserving heat and reacting for 6-10 hours until no distillate exists in the reaction, then cooling to 60 ℃, slowly dropwise adding 15 parts of cationic etherifying agent, controlling the temperature to be not more than 80 ℃, preserving heat for 5 hours at 70-80 ℃, then cooling to 50-60 ℃, slowly dropwise adding 5 parts of paraformaldehyde, controlling the temperature to be not more than 70 ℃, preserving heat for 4 hours at 70-80 ℃ after dropwise adding, and then cooling to 50-60 ℃ and discharging to obtain the cationic asphalt emulsifier.
Preparation of emulsified asphalt
The preparation procedure was the same as in example 2.
Asphalt emulsion performance test: see Table 9
TABLE 9
According to the grading range recommended in the micro-surfacing and slurry seal technical guidelines in China, an MS-3 grading standard is adopted in the test, and the emulsified asphalt mixture is tested: see the table 10 below for a review of the table,
| detecting items | Unit (B) | Standard of | Detection result | Test method |
| Mixing time (30 ℃ C.) | s | ≥120 | 60 | ISSA TB 113 |
| Demulsification time | min | -- | —— | T 0753-1993 |
| The cohesive force test is not less than | N.m | 30min1.2 | —— | T 0754-2011 |
Table 10
As indicated in tables 9-10, when the contents of several components do not meet the limit, the performance is significantly deteriorated: when the content of dimer is too much, the storage stability of emulsified asphalt is deteriorated, the mixing is fast, normal construction is affected, and when the content of dimer acid is too little, the demulsification time is too long, so that the cohesive force test is unqualified, and normal open traffic time is affected.
Claims (3)
1. The cationic asphalt emulsifier is characterized by comprising the following components in parts by weight:
20-30 parts of dimer acid, 5-20 parts of polyamine, 5-25 parts of cationic etherifying agent CHPTAC and 3-10 parts of paraformaldehyde; the dimer acid is dimer fatty acid, and the dimer fatty acid is one or more selected from linoleic acid dimer acid, palmitic acid dimer acid and dehydrated castor oil dimer acid; the polyamine is one or more of triethylene tetramine, tetraethylene pentamine, polyethylene polyamine and aminoethylpiperazine; the cationic etherifying agent is a 3-chloro-2-hydroxypropyl trimethyl ammonium chloride aqueous solution with the solid content of 50% -70%;
the preparation method of the cationic asphalt emulsifier comprises the following steps:
adding dimer acid into a four-mouth bottle, heating to 80 ℃, slowly adding polyamine into the four-mouth bottle, stirring, heating to 150 ℃ within half an hour, preserving heat for reaction for 6-10 hours, cooling to 60 ℃ until no distillate exists in the reaction, slowly dropwise adding a cationic etherifying agent, controlling the temperature to be not more than 80 ℃, preserving heat for 5 hours at 70-80 ℃ after dropwise adding, cooling to 50-60 ℃, slowly dropwise adding paraformaldehyde, controlling the temperature to be not more than 70 ℃, preserving heat for 4 hours at 70-80 ℃ after dropwise adding, cooling to 50-60 ℃ and discharging to obtain the asphalt emulsifier.
2. A method of preparing the cationic asphalt emulsifier of claim 1, comprising the steps of:
adding dimer acid into a four-mouth bottle, heating to 80 ℃, slowly adding polyamine into the four-mouth bottle, stirring, heating to 150 ℃ within half an hour, preserving heat for reaction for 6-10 hours, cooling to 60 ℃ until no distillate exists in the reaction, slowly dropwise adding a cationic etherifying agent, controlling the temperature to be not more than 80 ℃, preserving heat for 5 hours at 70-80 ℃ after dropwise adding, cooling to 50-60 ℃, slowly dropwise adding paraformaldehyde, controlling the temperature to be not more than 70 ℃, preserving heat for 4 hours at 70-80 ℃ after dropwise adding, cooling to 50-60 ℃ and discharging to obtain the asphalt emulsifier.
3. A method for preparing asphalt emulsion by using the cationic asphalt emulsifier of claim 1, which is characterized by comprising the following steps of preparing the cationic asphalt emulsifier into an aqueous solution accounting for 2.0-2.6% of the mass fraction of the asphalt emulsion, adjusting the pH value to 2-3 by using a hydrochloric acid solution, adding the cationic styrene-butadiene latex, and heating to 50-60 ℃; preheating a colloid mill to 50-60 ℃, adding asphalt at 120-140 ℃, and shearing and mixing by the colloid mill to obtain asphalt emulsion.
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| JP3957389B2 (en) * | 1998-02-13 | 2007-08-15 | 昭和シェル石油株式会社 | Asphalt emulsion |
| US7833338B2 (en) * | 2004-02-18 | 2010-11-16 | Meadwestvaco Packaging Systems, Llc | Method for producing bitumen compositions |
| CN102719106B (en) * | 2012-06-21 | 2014-03-26 | 河北工业大学 | Polyamine slow-breaking quick-setting asphalt emulsifier and preparation method and application thereof |
| CN103333136B (en) * | 2013-07-05 | 2015-07-22 | 河北工业大学 | Preparation method of polyaminoamide cationic asphalt emulsifier |
| CN105295068A (en) * | 2015-10-30 | 2016-02-03 | 华烁科技股份有限公司 | High-cation-degree asphalt emulsifier and application thereof |
| CN106589407B (en) * | 2016-12-15 | 2019-05-10 | 天津康泽威科技有限公司 | A kind of SBS modified pitch emulsifier and preparation method thereof and modified emulsifying asphalt product |
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