CN117701018B - Modified high-viscosity asphalt and preparation method thereof - Google Patents

Modified high-viscosity asphalt and preparation method thereof Download PDF

Info

Publication number
CN117701018B
CN117701018B CN202311509102.1A CN202311509102A CN117701018B CN 117701018 B CN117701018 B CN 117701018B CN 202311509102 A CN202311509102 A CN 202311509102A CN 117701018 B CN117701018 B CN 117701018B
Authority
CN
China
Prior art keywords
soybean oil
asphalt
epoxidized soybean
reaction
modified high
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202311509102.1A
Other languages
Chinese (zh)
Other versions
CN117701018A (en
Inventor
范佳明
李韶华
任振勇
许志勇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong Baicheng New Material Technology Co ltd
Original Assignee
Shandong Baicheng New Material Technology Co ltd
Filing date
Publication date
Application filed by Shandong Baicheng New Material Technology Co ltd filed Critical Shandong Baicheng New Material Technology Co ltd
Priority to CN202311509102.1A priority Critical patent/CN117701018B/en
Publication of CN117701018A publication Critical patent/CN117701018A/en
Application granted granted Critical
Publication of CN117701018B publication Critical patent/CN117701018B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention relates to the technical field of asphalt, and discloses modified high-viscosity asphalt and a preparation method thereof, wherein the invention uses 3- (dimethylamino) -1-propionamido butyric acid to catalyze by triphenylphosphine, and (3) carrying out ring opening esterification reaction with epoxy groups of the epoxidized soybean oil to obtain tertiary amine epoxidized soybean oil, and finally carrying out microwave-assisted reaction to carry out quaternization with alkyl chloride to obtain the cationic epoxidized soybean oil emulsifier. The hydroxyethyl cellulose is used as a tackifier, asphalt is added into emulsion of the cationic epoxy soybean oil emulsifier to form uniform oil-in-water emulsion, and the emulsion has the advantages of good emulsification condition, long emulsion stability time and high storage stability; the cationic epoxy soybean oil emulsifier contains nitrogen-containing groups such as quaternary ammonium salt and amide bond, and can prolong the adsorption process between asphalt and stone surface in the mixing process, thereby prolonging the mixing time, achieving the effect of slow cracking and quick setting and better meeting the construction requirements.

Description

Modified high-viscosity asphalt and preparation method thereof
Technical Field
The invention relates to the technical field of asphalt, in particular to modified high-viscosity asphalt and a preparation method thereof.
Background
Asphalt is a building material with wide application, and is mainly applied to the waterproof and anticorrosion fields of roofing, ground and underground structures. The emulsified asphalt has the advantages of good fluidity, strong cohesiveness, convenient construction and the like, and the emulsified asphalt heats and melts asphalt, forms fine particles through mechanical stirring, and is dispersed in an emulsifier solution to form the oil-in-water emulsion. The asphalt is mainly divided into cationic emulsified asphalt, anionic emulsified asphalt, nonionic emulsified asphalt and the like. The storage stability of emulsified asphalt is improved, the mixing time and other performances are prolonged, the construction requirements can be effectively met, and the patent CN103333136B discloses that polyethylene polyamine, formaldehyde, organic acid, quaternizing agent and the like are used as reaction raw materials to prepare the polyamine amide cationic asphalt emulsifier, and the emulsifier has the advantages of small using amount of the emulsifier and good stability. The invention aims to prepare the cationic epoxidized soybean oil emulsifier, improve the storage stability and the mixing time of emulsified asphalt and better meet the construction requirements.
Disclosure of Invention
The invention solves the following technical problems: the modified high-viscosity asphalt and the preparation method thereof are provided, the storage stability of the emulsified asphalt is improved, and the mixing time is prolonged.
The invention provides the following technical scheme:
A preparation method of modified high-viscosity asphalt comprises the following components, by weight, 100 parts of asphalt, 1.5-3 parts of cationic epoxy soybean oil emulsifier, 50-55 parts of water and 0.2-0.8 part of hydroxyethyl cellulose tackifier; the preparation method comprises the following steps:
(1) Adding N, N-dimethylformamide solvent, tertiary amine epoxidized soybean oil and alkyl chloride into a reaction bottle provided with a condensing tube, placing the reaction bottle into a microwave reactor for reaction, concentrating under reduced pressure, and washing with acetone to obtain a cationic epoxidized soybean oil emulsifier;
(2) Adding a cationic epoxidized soybean oil emulsifier and a hydroxyethyl cellulose tackifier into water, uniformly stirring to form emulsion, dropwise adding hydrochloric acid, and adding the emulsion into a colloid mill; and heating and melting the asphalt, adding the asphalt into a colloid mill, and shearing and emulsifying to obtain the modified high-viscosity asphalt.
Further, the proportion of tertiary amine epoxidized soybean oil and alkyl chloride in the step (1) is 1g (0.38-0.65 g); the molecular formula of the alkyl chloride is C nH2n+1 C l, and n is 4-12.
Further, the power of the microwave reactor in the reaction in the step (1) is 500-700W, the reaction temperature is 130-145 ℃ and the reaction time is 2-4h.
Further, the pH of the emulsion is regulated to 2-3 by dropwise adding hydrochloric acid in the step (2).
Further, (3) adding a solvent, 3- (dimethylamino) -1-propylamine and succinic anhydride into a reaction bottle, reacting for 2-4 hours at the temperature of 30-45 ℃, concentrating under reduced pressure, and washing with petroleum ether to obtain 3- (dimethylamino) -1-propionamidobutyric acid; the reaction formula is as follows:
(4) Adding 3- (dimethylamino) -1-propionamido butyric acid and triphenylphosphine into a reaction bottle, stirring for 10-20min, adding epoxidized soybean oil, stirring for reaction, and cooling to obtain tertiary amine epoxidized soybean oil.
Further, the solvent in (3) is any one of ethyl acetate, toluene, tetrahydrofuran or acetone.
Further, the proportion of 3- (dimethylamino) -1-propylamine and succinic anhydride in (3) is 1g (0.98-1.15 g).
Further, the ratio of 3- (dimethylamino) -1-propionamidobutyric acid, triphenylphosphine, epoxidized soybean oil in (4) is (0.5-0.7) g (0.16-0.24) g:1g.
Further, the reaction temperature in the step (4) is 120-135 ℃ and the reaction time is 5-10 h.
The invention has the following technical effects:
the preparation method comprises the steps of taking 3- (dimethylamino) -1-propylamine and succinic anhydride as reactants to obtain 3- (dimethylamino) -1-propionamido-butyric acid, then carrying out ring opening esterification reaction on carboxyl and epoxy groups of epoxy soybean oil under the catalysis of triphenylphosphine to obtain tertiary amine epoxy soybean oil, and finally carrying out microwave-assisted reaction to carry out quaternization with alkyl chloride to obtain the cationic epoxy soybean oil emulsifier.
According to the invention, hydroxyethyl cellulose is used as a tackifier, asphalt is added into emulsion of cationic epoxidized soybean oil emulsifier to form uniform oil-in-water emulsion, and the method has the advantages of good emulsification condition, long emulsion stability time and high storage stability, and simultaneously improves the properties of asphalt evaporant such as ductility, softening point and the like; the cationic epoxy soybean oil emulsifier contains nitrogen-containing groups such as quaternary ammonium salt and amide bond, and can prolong the adsorption process between asphalt and stone surface in the mixing process, thereby prolonging the mixing time, achieving the effect of slow cracking and quick setting and better meeting the construction requirements.
Detailed Description
In order to better understand the technical solutions of the present invention, the following description will clearly and completely describe the technical solutions of the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
Example 1
150ML of ethyl acetate solvent, 10g of 3- (dimethylamino) -1-propylamine and 10.7g of succinic anhydride are added into a reaction bottle to react for 2 hours at the temperature of 45 ℃, and then the mixture is decompressed, concentrated and washed by petroleum ether to obtain 3- (dimethylamino) -1-propionamidobutyric acid;
7.5g of 3- (dimethylamino) -1-propionamidobutyric acid and 2.4g of triphenylphosphine are added into a reaction flask, stirred for 10min, 15g of epoxidized soybean oil is added, stirred at 135 ℃ for 5h, and cooled to obtain tertiary amine epoxidized soybean oil.
Adding 5mL of N, N-dimethylformamide solvent, 4g of tertiary amine epoxy soybean oil and 1.52g of 1-chlorobutane into a reaction bottle provided with a condensing tube, placing the reaction bottle into a microwave reactor, controlling the power to be 600W, reacting for 2 hours at 145 ℃, concentrating under reduced pressure, washing with acetone, and obtaining the cationic epoxy soybean oil emulsifier;
Adding 7.5g of cationic epoxidized soybean oil emulsifier and 2g of hydroxyethyl cellulose tackifier into 250mL of water, uniformly stirring to form emulsion, dropwise adding hydrochloric acid to adjust the pH of the emulsion to 3, and adding the emulsion into a colloid mill; 500g of asphalt is heated and melted, then added into a colloid mill, sheared and emulsified to obtain the modified high-viscosity asphalt.
Example 2
Adding 200mL of acetone solvent, 10g of 3- (dimethylamino) -1-propylamine and 11.5g of succinic anhydride into a reaction bottle, reacting for 3 hours at 30 ℃, concentrating under reduced pressure, and washing with petroleum ether to obtain 3- (dimethylamino) -1-propionamidobutyric acid;
10.2g of 3- (dimethylamino) -1-propionamidobutyric acid and 2.8g of triphenylphosphine are added into a reaction flask, stirred for 20min, 15g of epoxidized soybean oil is added, stirred at 120 ℃ for reaction for 10h, and cooled to obtain tertiary amine epoxidized soybean oil.
Adding 8mL of N, N-dimethylformamide solvent, 4g of tertiary amine epoxy soybean oil and 1.88g of 1-chlorooctane into a reaction bottle provided with a condensing tube, placing the reaction bottle into a microwave reactor, controlling the power to be 500W, reacting for 2 hours at 145 ℃, concentrating under reduced pressure, washing with acetone, and obtaining the cationic epoxy soybean oil emulsifier;
Adding 10g of cationic epoxidized soybean oil emulsifier and 1g of hydroxyethyl cellulose tackifier into 250mL of water, uniformly stirring to form emulsion, dropwise adding hydrochloric acid to adjust the pH of the emulsion to 3, and adding the emulsion into a colloid mill; 500g of asphalt is heated and melted, then added into a colloid mill, sheared and emulsified to obtain the modified high-viscosity asphalt.
Example 3
Adding 100mL of toluene solvent, 10g of 3- (dimethylamino) -1-propylamine and 9.8g of succinic anhydride into a reaction bottle, reacting for 2 hours at the temperature of 45 ℃, concentrating under reduced pressure, and washing with petroleum ether to obtain 3- (dimethylamino) -1-propionamidobutyric acid;
12.7g of 3- (dimethylamino) -1-propionamidobutyric acid and 3.2g of triphenylphosphine are added into a reaction flask, stirred for 15min, 15g of epoxidized soybean oil is added, stirred at 130 ℃ for reaction for 8h, and cooled to obtain tertiary amine epoxidized soybean oil.
Adding 10mL of N, N-dimethylformamide solvent, 4g of tertiary amine epoxy soybean oil and 2.31g of 1-chlorodecane into a reaction bottle provided with a condensing tube, placing the reaction bottle into a microwave reactor, controlling the power to be 500W, reacting for 4 hours at 135 ℃, concentrating under reduced pressure, washing with acetone, and obtaining the cationic epoxy soybean oil emulsifier;
Adding 12.5g of cationic epoxidized soybean oil emulsifier and 4g of hydroxyethyl cellulose tackifier into 275mL of water, uniformly stirring to form emulsion, dropwise adding hydrochloric acid to adjust the pH of the emulsion to 2, and adding the emulsion into a colloid mill; 500g of asphalt is heated and melted, then added into a colloid mill, sheared and emulsified to obtain the modified high-viscosity asphalt.
Example 4
Adding 150mL of tetrahydrofuran solvent, 10g of 3- (dimethylamino) -1-propylamine and 11.5g of succinic anhydride into a reaction bottle, reacting for 4 hours at 35 ℃, concentrating under reduced pressure, and washing with petroleum ether to obtain 3- (dimethylamino) -1-propionamidobutyric acid;
15g of 3- (dimethylamino) -1-propionamidobutyric acid and 3.6g of triphenylphosphine are added into a reaction flask, stirred for 20min, 15g of epoxidized soybean oil is added, stirred at 135 ℃ for reaction for 6h, and cooled to obtain tertiary amine epoxidized soybean oil.
Adding 10mL of N, N-dimethylformamide solvent, 4g of tertiary amine epoxy soybean oil and 2.6g of 1-chlorododecane into a reaction bottle provided with a condensing tube, placing the reaction bottle into a microwave reactor, controlling the power to be 600W, reacting for 3 hours at 145 ℃, concentrating under reduced pressure, washing with acetone, and obtaining the cationic epoxy soybean oil emulsifier;
Adding 15g of cationic epoxidized soybean oil emulsifier and 3g of hydroxyethyl cellulose tackifier into 275mL of water, uniformly stirring to form emulsion, dropwise adding hydrochloric acid to adjust the pH of the emulsion to 3, and adding the emulsion into a colloid mill; 500g of asphalt is heated and melted, then added into a colloid mill, sheared and emulsified to obtain the modified high-viscosity asphalt.
Comparative example 1
Adding 7.5g of epoxidized soybean oil and 3g of hydroxyethyl cellulose tackifier into 250mL of water, uniformly stirring to form emulsion, dropwise adding hydrochloric acid to adjust the pH of the emulsion to 3, and adding the emulsion into a colloid mill; 500g of asphalt is heated and melted, then added into a colloid mill, sheared and emulsified to obtain the modified high-viscosity asphalt.
Asphalt performance was tested by reference to the JTJ052-2000 standard method.
TABLE 1 testing of the blendable time of modified high viscosity asphalt
Mixing time(s)
Example 1 265
Example 2 280
Example 3 310
Example 4 335
Comparative example 1 145
Table 2 table for performance test of modified high viscosity asphalt
Table 3 table of performance test of evaporation residue of modified high viscosity asphalt
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.

Claims (6)

1. The preparation method of the modified high-viscosity asphalt is characterized by comprising the following components in parts by weight: 100 parts of asphalt, 1.5-3 parts of cationic epoxy soybean oil emulsifier, 50-55 parts of water and 0.2-0.8 part of hydroxyethyl cellulose tackifier; the preparation method comprises the following steps:
(1) Adding N, N-dimethylformamide solvent, tertiary amine epoxidized soybean oil and alkyl chloride into a reaction bottle provided with a condensing tube, placing the reaction bottle into a microwave reactor for reaction, concentrating under reduced pressure, and washing with acetone to obtain a cationic epoxidized soybean oil emulsifier;
(2) Adding a cationic epoxidized soybean oil emulsifier and a hydroxyethyl cellulose tackifier into water, uniformly stirring to form emulsion, dropwise adding hydrochloric acid, and adding the emulsion into a colloid mill; heating and melting asphalt, adding the asphalt into a colloid mill, and shearing and emulsifying to obtain modified high-viscosity asphalt;
the preparation method of the tertiary amine epoxidized soybean oil comprises the following steps:
S1, adding a solvent, 3- (dimethylamino) -1-propylamine and succinic anhydride into a reaction bottle, reacting for 2-4 hours at the temperature of 30-45 ℃, concentrating under reduced pressure, and washing with petroleum ether to obtain 3- (dimethylamino) -1-propionamidobutyric acid;
S2, adding 3- (dimethylamino) -1-propionamido butyric acid and triphenylphosphine into a reaction bottle, stirring for 10-20min, adding epoxidized soybean oil, stirring for reaction, and cooling to obtain tertiary amine epoxidized soybean oil;
the proportion of 3- (dimethylamino) -1-propylamine and succinic anhydride in the S1 is 1g (0.98-1.15 g);
The proportion of 3- (dimethylamino) -1-propionamidobutyric acid, triphenylphosphine and epoxidized soybean oil in the S2 is (0.5-0.7) g (0.16-0.24) g and 1g.
2. The method for preparing modified high-viscosity asphalt according to claim 1, wherein the proportion of tertiary amine epoxidized soybean oil and alkyl chloride in (1) is 1g (0.38-0.65) g; the molecular formula of the alkyl chloride is C nH2n+1 Cl, and n is 4-12.
3. The method for preparing modified high-viscosity asphalt according to claim 1, wherein the power of the microwave reactor in the reaction in the step (1) is 500-700W, the reaction temperature is 130-145 ℃ and the time is 2-4h.
4. The method for producing a modified high-viscosity asphalt according to claim 1, wherein the pH of the emulsion is adjusted to 2 to 3 by dropping hydrochloric acid into the (2).
5. The method for preparing modified high-viscosity asphalt according to claim 1, wherein the solvent in S1 is any one of ethyl acetate, toluene, tetrahydrofuran or acetone.
6. The method for preparing modified high-viscosity asphalt according to claim 1, wherein the reaction temperature in S2 is 120-135 ℃ for 5-10 hours.
CN202311509102.1A 2023-11-14 Modified high-viscosity asphalt and preparation method thereof Active CN117701018B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311509102.1A CN117701018B (en) 2023-11-14 Modified high-viscosity asphalt and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311509102.1A CN117701018B (en) 2023-11-14 Modified high-viscosity asphalt and preparation method thereof

Publications (2)

Publication Number Publication Date
CN117701018A CN117701018A (en) 2024-03-15
CN117701018B true CN117701018B (en) 2024-09-24

Family

ID=

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106633102A (en) * 2016-11-22 2017-05-10 汪逸凡 Preparation method of high-stability composite cationic asphalt emulsifier
CN111423734A (en) * 2020-04-13 2020-07-17 湖南大学 Reactive type regenerated SBS (styrene butadiene styrene) modified asphalt and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106633102A (en) * 2016-11-22 2017-05-10 汪逸凡 Preparation method of high-stability composite cationic asphalt emulsifier
CN111423734A (en) * 2020-04-13 2020-07-17 湖南大学 Reactive type regenerated SBS (styrene butadiene styrene) modified asphalt and preparation method thereof

Similar Documents

Publication Publication Date Title
CN101745340B (en) Cationic asphalt emulsifier and preparation method and application thereof
JP2592574B2 (en) Curing agent for aqueous epoxy resin dispersion and method for producing the same
DE69927734T2 (en) Curable resin composition
CN103012180B (en) Preparation method of organic rheology modifying agent for full-oil-based drilling fluid
JP3391074B2 (en) Epoxy resin composition
CN101624385A (en) Non-ionic self-emulsifying aqueous epoxy hardener and preparation method and application thereof
US5443632A (en) Cationic aqueous bituminous emulsion-aggregate slurries
US5352285A (en) Microsurfacing system
KR101243511B1 (en) Microcapsule-type latent curing agent for epoxy resin and process for production thereof, and one-pack-type epoxy resin composition and cured product thereof
NL2026927B1 (en) A silicone-modified vegetable oil-based polyol as well as its preparation method and application
CN102976649B (en) Warm-mixing agent used for waste-rubber-powder-modified asphalt, and preparation method thereof
CN117701018B (en) Modified high-viscosity asphalt and preparation method thereof
CN103224612A (en) Solvent-free self-leveling epoxy resin curing agent and preparation method thereof
CN113860759A (en) Preparation method of basalt fiber impregnating compound with water-based polyurethane as film forming agent
CN102675861A (en) Single-component water-based epoxy resin emulsion and preparation method thereof
CN117701018A (en) Modified high-viscosity asphalt and preparation method thereof
CN104761917B (en) A kind of organic composite warm-mixed asphalt and preparation method thereof
JPH02227470A (en) Epoxy resin powder coating composition
JPH0315654B2 (en)
JP3493239B2 (en) Method for producing asphalt emulsion
CN108467495A (en) A kind of lignin quaternary ammonium salt cation asphalt emulsifier and preparation method thereof
CN108517040A (en) A kind of cellulose family quaternary ammonium salt cation asphalt emulsifier and preparation method thereof
CN109694481B (en) Carboxylic acid bis-quaternary ammonium salt type sodium hydroxypropyl phosphate asphalt emulsifier and preparation method thereof
CN107189458B (en) Modified asphalt with thermal storage stability and preparation method thereof
CN111848980B (en) Asphalt emulsifier containing ester-based polyamine quaternary ammonium salt, emulsified asphalt and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
SE01 Entry into force of request for substantive examination
GR01 Patent grant