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Technology for synthesizing bisquaternary ammonium salt slow-breaking quick-setting asphalt emulsifier

A technology of asphalt emulsifier and double quaternary ammonium salt, which is applied in chemical instruments and methods, chemical/physical processes, building components, etc., can solve problems such as little room for improvement, limited source of emulsifier raw materials, complicated process, etc., to achieve Uniform and fine asphalt emulsion particles, slow cracking and fast setting performance, and good storage stability

Inactive Publication Date: 2012-07-18
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patent USP4338136 has reported a kind of emulsifier prepared by the reaction of long-chain fatty acid and diethylenetriamine, and the shortcoming of this emulsifier is that when being used for slurry sealing layer construction, the demulsification time is long, and the molding time is slow; US5443632 reports a A slow-cracking and fast-setting cationic emulsifier, which is obtained by reacting polyamine condensation products of fatty acids or resins with quaternary ammonium agents
The disadvantage of this method is that it is expensive and there is little room for product improvement; USP5137572 reports a new type of cationic asphalt emulsifier, which has strong flexibility in use, and can adapt to complex and changeable formulations and processes during preparation However, due to the complex process of this method, the limited source of raw materials and the high price, the popularization and application are greatly restricted; CN101712625 reports a new type of amphoteric slow-cracking and fast-setting asphalt emulsifier, which is generated by the reaction of oleic acid and polyamines Prepared by the halogenation reaction of amidopolyamine and chloroacetic acid
This emulsifier expands the selectivity to stone material in the slurry seal layer, but this emulsifier lacks flexibility in the design of molecular structure, has limitation in adapting to the asphalt emulsification of different structures and places of production; CN1861721 reports that by rosin A rosin-type cationic asphalt emulsifier prepared by condensing rosin intermediates with alkenyl polyamines, and then condensed with quaternary ammonium salt intermediates. The disadvantage of this emulsifier is that it needs to be modified before it can be used for slurry sealing, and the product is not practical. Too ideal; CN1096714 reported a kind of asphalt emulsifier prepared by naphthenic acid and alkenyl polyamine, but the shortcoming of this method is that the raw material source of emulsifier is limited, can't effectively improve product performance

Method used

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  • Technology for synthesizing bisquaternary ammonium salt slow-breaking quick-setting asphalt emulsifier
  • Technology for synthesizing bisquaternary ammonium salt slow-breaking quick-setting asphalt emulsifier
  • Technology for synthesizing bisquaternary ammonium salt slow-breaking quick-setting asphalt emulsifier

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Preparation of emulsifier: 16.3g octadecyl-1,3-propylenediamine, 7.0g oleic acid, 7.4g cinnamic acid, 1.0g p-toluenesulfonic acid, 20g xylene were added to the reaction vessel, Stir and reflux reaction at 125°C for 4 hours, distill off the xylene, cool down to 65°C, add 20g of isopropanol to obtain the amide intermediate;

[0021] Mix 5.1g of triethylamine and 5g of concentrated hydrochloric acid uniformly at 40°C, then dropwise add 4.6g of epichlorohydrin into the reaction vessel, stir and react at 45°C for 4h, cool to room temperature, and obtain the quaternary ammonium salt intermediate;

[0022] Add the quaternary ammonium salt intermediate prepared above dropwise to the amide intermediate prepared above at 80-85°C, and stir and react at this temperature for 4 hours to obtain a double quaternary ammonium salt type cationic asphalt emulsifier product.

[0023] Preparation of emulsifier aqueous solution: Dissolve 2.0g of the emulsifier in 100g of warm water, heat the ...

Embodiment 2

[0032] Emulsifier preparation: Add 13.5g octadecylamine, 5.8g maleic acid, 5.0g lauric acid, 1.0g p-toluenesulfonic acid, 20g xylene into the reaction vessel, and stir and reflux at 110°C for 4h Distill out xylene, lower the temperature to 65°C, add 20g of isopropanol to obtain the amide intermediate;

[0033] Mix 15g of octadecyldimethylamine and 5g of concentrated hydrochloric acid at 45°C, then drop 4.6g of epichlorohydrin into the reaction vessel, react at 50-55°C for 4h, cool to room temperature, and obtain quaternary ammonium salt Intermediate;

[0034] The quaternary ammonium salt intermediate prepared above was added dropwise to the amide intermediate prepared above at 80-85°C, and stirred and reacted at this temperature for 4 hours to obtain a double quaternary ammonium salt type cationic asphalt emulsifier product.

[0035] Preparation of emulsifier aqueous solution: Add 2.0g of the emulsifier into 100g of hot water at 65-80°C. After the emulsifier is dissolved, adj...

Embodiment 3

[0040] Preparation of emulsifier: 16.3g of N-octadecylpropylenediamine, 9g of abietic acid, 5.7g of stearic acid, 1.0g of p-toluenesulfonic acid, and 20g of trimethylbenzene were added to the reaction vessel and refluxed at 140°C After reacting for 4 hours, trimethylbenzene was distilled off, the temperature was lowered to 65°C, and 20 g of isopropanol was added to obtain the amide intermediate;

[0041] Mix 9g of octadecyldimethylamine, 2g of triethylamine and 5g of concentrated hydrochloric acid at 40°C, then dropwise add 4.6g of epichlorohydrin into the reaction vessel, stir and react at 45-50°C for 4h to obtain quaternary Ammonium salt intermediate;

[0042]Add the quaternary ammonium salt intermediate prepared above dropwise to the amide intermediate prepared above at 75~80°C, and stir and react at this temperature for 4 hours to obtain the double quaternary ammonium salt type cationic asphalt emulsifier product.

[0043] Preparation of emulsifier aqueous solution: Add 2...

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Abstract

The invention relates to a technology for synthesizing a bisquaternary ammonium salt slow-breaking quick-setting asphalt emulsifier. The technology comprises the steps of: (1) adding mixed fatty acid, long-chain aliphatic amine, an aromatic hydrocarbon solvent and a catalyst in a reaction vessel for backflow reaction, then removing the solvent through reduced pressure distillation, cooling and adding an alcohol solvent to obtain an amide or multi-acyl amide intermediate; (2) mixing aliphatic tertiary amine with hydrochloric acid, then dripping epoxy chloropropane, mixing for a reaction and cooling to a room temperature to obtain a quaternary ammonium salt intermediate; and (3) dripping the quaternary ammonium salt intermediate into the amide or multi-acyl amide intermediate for reaction so as to obtain the bisquaternary ammonium salt type cationic asphalt emulsifier. The technology for synthesizing the bisquaternary ammonium salt slow-breaking quick-setting asphalt emulsifier, disclosed by the invention, has the advantages of wide raw material source, high cost performance, wide application range and convenience in popularization and application. The asphalt emulsion has uniform and fine particles and good storage stability; and wide slow-breaking quick-setting use performances can be obtained.

Description

technical field [0001] The invention relates to the field of fine organic chemicals, in particular to a synthesis process of a double quaternary ammonium salt slow-cracking and fast-setting asphalt emulsifier. The cationic asphalt emulsion prepared by using this emulsifier has good water solubility, high storage stability and Wide application characteristics. Background technique [0002] Petroleum bitumen is a common raw material in transportation construction and some other industries. In the early 20th century, petroleum asphalt developed rapidly as a road engineering material, its variety and quality continued to improve, and its application range became wider and wider. However, during the use of road asphalt, in order to maintain the fluidity of the asphalt, a large amount of energy will be consumed, and problems such as environmental pollution will occur. Emulsified asphalt, especially cationic emulsified asphalt, has many excellent properties and characteristics su...

Claims

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Application Information

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IPC IPC(8): B01F17/18B01F17/22B01F17/38C08L95/00C09K23/18C09K23/22C09K23/38
Inventor 靳素荣庞金兴韩秀邱辉刘军黄红明
Owner WUHAN UNIV OF TECH
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