CN108070007B - Asphalt emulsifier for cold recycling and preparation method thereof - Google Patents
Asphalt emulsifier for cold recycling and preparation method thereof Download PDFInfo
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- CN108070007B CN108070007B CN201711315396.9A CN201711315396A CN108070007B CN 108070007 B CN108070007 B CN 108070007B CN 201711315396 A CN201711315396 A CN 201711315396A CN 108070007 B CN108070007 B CN 108070007B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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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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- Engineering & Computer Science (AREA)
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- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
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Abstract
The invention provides an asphalt emulsifier for cold recycling and a preparation method thereof. The method comprises the following operation steps: (1) carrying out high-temperature reflux reaction on fatty acid, maleic anhydride and a catalyst to obtain an intermediate; (2) uniformly stirring acetone and mixed amine, adding sodium carbonate, dropwise adding epoxy chloropropane, and stirring for reaction; (3) adding lignin into the reaction liquid in the step (2), and dehydrating at high temperature; (4) adding fatty acid into the reaction liquid in the step (3), stirring at high temperature for dehydration, adding the product intermediate in the step (1), and stirring at high temperature for dehydration; (5) and (4) cooling the product obtained in the step (4), adding water, dropwise adding acrylic acid, uniformly stirring, heating for dehydration, cooling, and adjusting the solid content to obtain the asphalt emulsifier for cold recycling. The asphalt emulsifier for cold recycling prepared by the invention has stronger emulsifying capacity, the prepared emulsified asphalt has good storage stability, and is uniformly coated with waste stone; the road performance indexes of the corresponding cold-recycling mixed material are all superior to the national standard.
Description
Technical Field
The invention relates to an asphalt emulsifier for cold regeneration, and in particular relates to a preparation method of a lignin asphalt emulsifier for cold regeneration.
Background
With the rapid development of highway construction in China, the asphalt pavement needing to be renovated is rapidly increased every year. If a large amount of the dug and milled asphalt mixture is discarded, the environment is polluted, resources are wasted, and the ecological environment is damaged by exploiting new stones. The cold regeneration technology can save energy and resources, 100% utilize the old asphalt mixture, prolong the construction season, improve the working conditions of constructors and reduce the environmental pollution. At present, the cold recycling technology of emulsified asphalt in China is not mature, most cold recycling construction is only applied to a base layer or a lower surface layer, the quality of the recycled pavement of a few upper surface layers is difficult to reach the quality standard of an asphalt surface layer, and a comprehensive and detailed method and evaluation standard are lacked as references in actual construction application and laboratory research, so that the problems seriously restrict the large-scale application of the cold recycling technology of emulsified asphalt.
Lignin is an important component in paper-making wastewater, and thus, the amount of lignin produced by paper-making is as high as 450 million tons every year. So far, only about 6 percent of industrial lignin is utilized in China, and the rest is directly discharged into rivers or burnt along with waste water, which not only causes great waste of resources, but also seriously pollutes the environment. The asphalt emulsifier suitable for the cold regeneration system is mainly lignin, so that the lignin produced in the paper industry is used as the raw material of the cold regeneration emulsifier, resources can be saved, the environment can be protected, and the asphalt emulsifier has important significance for promoting the implementation of the strategy of energy conservation and emission reduction in China.
Disclosure of Invention
The invention aims to provide an emulsifier for cold recycling, which has strong emulsifying capacity, high storage stability, strong wrapping performance with old aggregates and good pavement performance, and a preparation method thereof.
The preparation method of the emulsifier provided by the invention comprises the following steps:
(1) adding 20-40 parts by mass of maleic anhydride and 0.15-0.5 part by mass of catalyst into 100 parts by mass of fatty acid, slowly heating to 210 ℃ and 240 ℃, and stirring for reaction for 2-5 hours to obtain an intermediate;
(2) weighing 10-20 parts by mass of acetone, placing the acetone into a reaction container, adding 100 parts by mass of mixed amine, uniformly stirring, adding 3-6 parts by mass of sodium carbonate, uniformly stirring, slowly dropwise adding 10-20 parts by mass of epoxy chloropropane, and reacting for 0.5-1h under stirring;
(3) adding 30-60 parts by mass of lignin into the reaction liquid in the step (2), heating to 150 ℃ and 200 ℃, and carrying out dehydration reaction for 0.5-3 h;
(4) adding 25-45 parts by mass of fatty acid into the reaction liquid in the step (3), stirring and dehydrating at 180 ℃ and 200 ℃ for 0.5-1h, adding 15-40g of intermediate, and stirring and dehydrating at 210 ℃ and 240 ℃ for 2-5 h;
(5) and (3) cooling the product obtained in the step (4) to 80-120 ℃, adding 5-10 parts by mass of tap water, uniformly stirring, dropwise adding 9-20 parts by mass of acrylic acid, uniformly stirring, heating to 180 ℃, reacting for 0.5-1h, cooling, and adjusting the solid content by using a solvent to obtain the asphalt emulsifier for cold regeneration.
In the step (1), the fatty acid is one of tall oil fatty acid, stearic acid, palmitic acid, oleic acid and abietic acid.
In the step (1), the catalyst is one of iodine, anhydrous aluminum chloride and clay, and in order to promote the maleic anhydride to be dissolved in the fatty acid, the maleic anhydride and the catalyst are added simultaneously.
And (3) the amine mixed solution in the step (2) is two of trimethylamine, triethylamine, diethylenetriamine, triethylene tetramine, tetraethylenepentamine and N-aminoethyl piperazine.
And (4) cooling the reaction product to 80-120 ℃, wherein the added solvent is one of ethylene glycol, diethylene glycol, triethylene glycol, n-butanol, isopropanol or methanol.
The innovation points of the invention are as follows: the amidation reaction of tricarboxylic acid, lignin and fatty acid exists in the synthesis of the cold-recycling asphalt emulsifier, so that the emulsifier has strong emulsifying capacity, and the corresponding emulsified asphalt has good stability and stone coating performance; the reaction of polyamine and acrylic acid with epichlorohydrin to generate amide is adopted for modification, thus achieving the dual purposes of improving the emulsifying capacity of the emulsifier and reducing the synthesis cost of the emulsifier.
The raw materials involved in the invention are easy to obtain, and the lignin can be effectively utilized. The obtained emulsifier has strong emulsifying capacity, the corresponding emulsified asphalt has good stability and good wrapping property with waste asphalt, and all road performances meet the technical indexes of the standard and the mixing performance of the cation emulsified asphalt.
Detailed Description
The process, emulsifying properties, emulsified asphalt and related properties of the emulsifier preparation method provided by the present invention will be further described with reference to the following examples, which are not intended to limit the present invention.
Example 1
Preparation of emulsifiers
Adding 20g of maleic anhydride and 0.15g of iodine into 100g of tall oil fatty acid, heating to 210 ℃, and reacting for 3h to obtain an intermediate. Weighing 10g of acetone, placing the acetone into a reaction container, adding 100g of trimethylamine and N-aminoethyl piperazine, uniformly stirring, adding 3g of sodium carbonate, uniformly stirring, slowly dropwise adding 10g of epoxy chloropropane, reacting for 0.5h while stirring, adding 60g of lignin, heating to 150 ℃, and performing dehydration reaction for 0.5 h. Adding 25g of tall oil fatty acid, heating to 180 ℃, carrying out dehydration reaction for 0.5h, adding 15g of intermediate, heating to 210 ℃, and carrying out dehydration reaction for 2 h. Cooling to 80 ℃, adding 5g of tap water, dropwise adding 9g of acrylic acid after uniformly stirring, heating to 180 ℃ after uniformly stirring, reacting for 0.5h, cooling to 80 ℃, and adjusting the solid content to 70% by using ethylene glycol.
Preparation of emulsified asphalt
10g of emulsifier is dissolved in 190g of water, and after uniform stirring, the pH value of the solution is adjusted to about 2.0 by concentrated hydrochloric acid. And starting the colloid mill, pouring the emulsifier aqueous solution heated to 60 ℃ into the colloid mill for circulation, slowly pouring 300g of asphalt heated to 130-140 ℃ into the colloid mill, and continuously circulating lmin to obtain the emulsified asphalt.
Asphalt emulsion performance index
Example 2
Preparation of emulsifiers
Adding 30g of maleic anhydride and 0.27g of iodine into 100g of tall oil fatty acid, heating to 220 ℃, and reacting for 4 hours to obtain an intermediate. Weighing 15g of acetone, placing the acetone into a reaction container, adding 100g of a mixture of diethylenetriamineand N-aminoethyl piperazine, uniformly stirring, adding 4.5g of sodium carbonate, uniformly stirring, slowly dropwise adding 15g of epoxy chloropropane, stirring for reacting for 1h, adding 45g of lignin, heating to 180 ℃, and performing dehydration reaction for 1 h. Adding 35g of tall oil fatty acid, heating to 200 ℃, carrying out dehydration reaction for 1h, adding 20g of intermediate, heating to 230 ℃, and carrying out dehydration reaction for 4 h. Cooling to 80 ℃, adding 7g of tap water, dropwise adding 15g of acrylic acid after uniformly stirring, heating to 180 ℃ after uniformly stirring, reacting for 1h, cooling to 120 ℃, and adjusting the solid content to 70% by using ethylene glycol.
Preparation of emulsified asphalt
10g of emulsifier is dissolved in 190g of water, and after uniform stirring, the pH value of the solution is adjusted to about 2.0 by concentrated hydrochloric acid. And starting the colloid mill, pouring the emulsifier aqueous solution heated to 60 ℃ into the colloid mill for circulation, slowly pouring 300g of asphalt heated to 130-140 ℃ into the colloid mill, and continuously circulating lmin to obtain the emulsified asphalt.
Asphalt emulsion performance index
Example 3
Preparation of emulsifiers
Adding 40g of maleic anhydride and 0.4g of iodine into 100g of tall oil fatty acid, heating to 230 ℃, and reacting for 5 hours to obtain an intermediate. Weighing 20g of acetone, placing the acetone into a reaction container, adding 100g of mixed solution of triethylene tetramine and N-aminoethyl piperazine, uniformly stirring, adding 6g of sodium carbonate, uniformly stirring, slowly dropwise adding 20g of epoxy chloropropane, stirring for reacting for 1 hour, adding 30g of lignin, heating to 200 ℃, and performing dehydration reaction for 2 hours. Adding 45g of tall oil fatty acid, heating to 200 ℃, carrying out dehydration reaction for 1h, adding 25g of intermediate, heating to 240 ℃, and carrying out dehydration reaction for 5 h. Cooling to 80 ℃, adding 9g of tap water, dropwise adding 20g of acrylic acid after uniformly stirring, heating to 180 ℃ after uniformly stirring, reacting for 1h, cooling to 120 ℃, and adjusting the solid content to 70% by using ethylene glycol.
Preparation of emulsified asphalt
10g of emulsifier is dissolved in 190g of water, and after uniform stirring, the pH value of the solution is adjusted to about 2.0 by concentrated hydrochloric acid. And starting the colloid mill, pouring the emulsifier aqueous solution heated to 60 ℃ into the colloid mill for circulation, slowly pouring 300g of asphalt heated to 130-140 ℃ into the colloid mill, and continuously circulating lmin to obtain the emulsified asphalt.
Asphalt emulsion performance index
Example 4
Preparation of emulsifiers
Adding 35g of maleic anhydride and 0.27g of iodine into 100g of tall oil fatty acid, heating to 240 ℃, and reacting for 4 hours to obtain an intermediate. Weighing 15g of acetone, placing the acetone into a reaction container, mixing 100g of tetraethylenepentamine and N-aminoethyl piperazine, uniformly stirring, adding 4.5g of sodium carbonate, uniformly stirring, slowly dropwise adding 15g of epoxy chloropropane, stirring for reacting for 1h, adding 45g of lignin, heating to 180 ℃, and performing dehydration reaction for 1 h. Adding 35g of tall oil fatty acid, heating to 200 ℃, carrying out dehydration reaction for 1h, adding 20g of intermediate, heating to 210 ℃, and carrying out dehydration reaction for 4 h. Cooling to 80 ℃, adding 8g of tap water, dropwise adding 17g of acrylic acid after uniformly stirring, heating to 180 ℃ after uniformly stirring, reacting for 1h, cooling to 120 ℃, and adjusting the solid content to 70% by using diethylene glycol.
Preparation of emulsified asphalt
10g of emulsifier is dissolved in 190g of water, and after uniform stirring, the pH value of the solution is adjusted to about 2.0 by concentrated hydrochloric acid. And starting the colloid mill, pouring the emulsifier aqueous solution heated to 60 ℃ into the colloid mill for circulation, slowly pouring 300g of asphalt heated to 130-140 ℃ into the colloid mill, and continuously circulating lmin to obtain the emulsified asphalt.
Asphalt emulsion performance index
Claims (4)
1. The preparation method of the asphalt emulsifier for cold recycling is characterized by comprising the following specific operation steps:
(1) adding 20-40 parts by mass of maleic anhydride and 0.15-0.5 part by mass of catalyst into 100 parts by mass of fatty acid, slowly heating to 210 ℃ and 240 ℃, and stirring for reaction for 2-5 hours to obtain an intermediate;
(2) weighing 10-20 parts by mass of acetone, placing the acetone into a reaction container, adding 100 parts by mass of mixed amine, uniformly stirring, adding 3-6 parts by mass of sodium carbonate, uniformly stirring, slowly dropwise adding 10-20 parts by mass of epoxy chloropropane, and reacting for 0.5-1h under stirring;
(3) adding 30-60 parts by mass of lignin into the reaction liquid in the step (2), heating to 150 ℃ and 200 ℃, and carrying out dehydration reaction for 0.5-3 h;
(4) adding 25-45 parts by mass of fatty acid into the reaction liquid in the step (3), stirring and dehydrating at 180 ℃ and 200 ℃ for 0.5-1h, adding 15-40g of intermediate, and stirring and dehydrating at 210 ℃ and 240 ℃ for 2-5 h;
(5) cooling the product obtained in the step (4) to 80-120 ℃, adding 5-10 parts by mass of tap water, uniformly stirring, dropwise adding 9-20 parts by mass of acrylic acid, uniformly stirring, heating to 180 ℃, reacting for 0.5-1h, cooling, and adjusting the solid content by using a solvent to obtain the asphalt emulsifier for cold regeneration;
the mixed amine in the step (2) is two or more of diethylenetriamine, triethylene tetramine, tetraethylene pentamine, piperazine and N-aminoethyl piperazine.
2. The method according to claim 1, wherein the fatty acid in the step (1) is one of tall oil fatty acid, stearic acid, palmitic acid, oleic acid and rosin acid.
3. The method according to claim 1, wherein the catalyst in the step (1) is one of iodine, anhydrous aluminum chloride and clay.
4. The method according to claim 1, wherein the solvent in the step (5) is one of ethylene glycol, diethylene glycol, triethylene glycol, n-butanol, isopropanol or methanol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711315396.9A CN108070007B (en) | 2017-12-12 | 2017-12-12 | Asphalt emulsifier for cold recycling and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109181130B (en) * | 2018-07-24 | 2021-07-30 | 上海舜雅化工有限公司 | Anionic oxidized polyethylene wax emulsion and preparation method and application thereof |
| CN111138685B (en) * | 2019-12-30 | 2022-07-01 | 湖南云中再生科技股份有限公司 | Emulsifier for cold recycling and preparation method thereof |
| TR202010383A2 (en) * | 2020-07-01 | 2021-05-21 | Ak Kim Kimya Sanayi Ve Ticaret Anonim Sirketi | WASTE OIL COLD ASPHALT ADDITIVE |
| CN113336964B (en) * | 2021-06-12 | 2023-11-17 | 河南金欧特实业集团股份有限公司 | Modified emulsified asphalt for normal temperature cold state asphalt pavement and preparation method thereof |
| CN114539556B (en) * | 2022-02-24 | 2023-11-10 | 西安博望新材料科技有限公司 | Emulsifier for cold-mixed high-viscosity emulsified asphalt and preparation method thereof |
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| CN102558575B (en) * | 2012-02-06 | 2013-10-30 | 陕西师范大学 | Preparation method for fatty acid derivate cation asphalt emulsifying agent |
| CN104530445B (en) * | 2014-12-16 | 2016-09-07 | 辽宁路通化工有限公司 | A kind of preparation method splitting fast solidifying type asphalt emulsifier slowly |
| CN106084250B (en) * | 2016-06-22 | 2018-06-12 | 山东大学 | A kind of lignin cyclammonium cationoid type asphalt emulsifier and preparation method thereof |
| CN106146861A (en) * | 2016-07-11 | 2016-11-23 | 江苏中路新材料科技发展有限公司 | A kind of preparation method of cold recycled asphalt emulsifying agent |
| CN106750374B (en) * | 2016-12-15 | 2019-05-10 | 天津康泽威科技有限公司 | A kind of asphalt emulsifier and preparation method thereof and emulsified asphalt product |
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