A kind of carboxylic acid diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier and its preparation method

A technology of sodium hydroxypropyl sulfonate and asphalt emulsifier, which is applied in the preparation of sulfonate, the preparation of cyanide reaction, chemical instruments and methods, etc. The effect of enhancing charge strength, improving emulsifying performance, and increasing hydrophilicity

Inactive Publication Date: 2018-07-10
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The general disadvantages of the above cationic asphalt emulsifiers and their preparation methods are: the cost of raw materials for the preparation of emulsifiers is high, the sources are limited, high temperature reactions are required during preparation, and the requirements for production and experimental equipment are relatively high
[0008] In summary, in the process of developing new asphalt emulsifiers, due to the unpredictability of the emulsifying properties of the reaction raw materials and prepared asphalt emulsifiers, this greatly increases the difficulty of developing new asphalt emulsifiers

Method used

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  • A kind of carboxylic acid diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier and its preparation method
  • A kind of carboxylic acid diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier and its preparation method
  • A kind of carboxylic acid diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier and its preparation method

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preparation example Construction

[0050] In one embodiment of the present invention, the preparation method of above-mentioned carboxylic acid diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier is provided, comprising the steps of:

[0051] (1) Add N-hydrogenated tallow-1,3-propylenediamine into the reaction vessel, add alcohol solvent, heat and stir to dissolve, then add acrylic acid in batches, after the addition, stir the reaction at 60-80°C 2-4h, obtain reaction intermediate I;

[0052] (2) Add sodium bisulfite to another reaction vessel, add water, heat and stir to dissolve, then add epichlorohydrin in batches, after the addition, stir and react at 40-85°C for 3-6h to obtain a reaction intermediate II (sodium 3-chloro-2-hydroxypropyl sulfonate);

[0053] (3) Add the reaction intermediate II to the reaction intermediate I in batches, and react at 60-80° C. for 3-6 hours to obtain a bisquaternary ammonium carboxylic acid sodium hydroxypropyl sulfonate asphalt emulsifier.

[...

Embodiment 1

[0062] (1) Preparation of carboxylic acid diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier:

[0063] 1) Add 326.0g of N-hydrogenated tallow-1,3-propylenediamine and 330g of isopropanol into the reactor, heat and stir to dissolve. Then gradually add 219.8g of acrylic acid, and stir at 70°C for 3h.

[0064] 2) Add 245.2g of sodium bisulfite and 785.4g of water into another reactor, stir to dissolve, and heat to 75°C. Then 197.8 g of epichlorohydrin was added dropwise, and stirred at 75° C. for 3.5 h to obtain an aqueous solution of 3-chloro-2-hydroxypropyl sulfonate sodium.

[0065] The above synthetic intermediate product was separated and purified by recrystallization and then detected by FTIR. The results are as follows: 3592cm -1 and 3522cm -1 It is free O-H stretching vibration absorption peak, 3362cm -1 It is the absorption peak of association O-H stretching vibration, 2923cm -1 It is the asymmetric stretching vibration absorption peak...

Embodiment 2

[0077] (1) Preparation of carboxylic acid diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier:

[0078] 1) Add 326.0g of N-hydrogenated tallow-1,3-propylenediamine and 330g of absolute ethanol into the reactor, heat and stir to dissolve. Then gradually add 219.8g of acrylic acid, and stir at 70°C for 3h.

[0079] 2) Add 245.2g of sodium bisulfite and 785.4g of water into another reactor, stir to dissolve, and heat to 75°C. Then 197.8 g of epichlorohydrin was added dropwise, and stirred at 75° C. for 3.5 h to obtain an aqueous solution of 3-chloro-2-hydroxypropyl sulfonate sodium.

[0080] 3) The aqueous solution of sodium 3-chloro-2-hydroxypropyl sulfonate prepared in step 2) was added dropwise to the synthesis product in the above step 1), and stirred at 75° C. for 3 h. Obtain carboxylic acid diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier, and keep it as emulsified asphalt test.

[0081] (2) Preparation of emul...

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Abstract

The invention discloses a carboxylic acid diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier, the molecular structure of which is as follows: it is prepared from raw materials with the following molar ratio: N-hydrogenated tallow-1,3- The molar ratio of propylene diamine, alcohol solvent, acrylic acid, epichlorohydrin, sodium bisulfite is 1mol: (5.00‑11.00) mol: (3.00‑3.10) mol: (2.00‑2.30) mol: (2.10‑ 2.50) mol. The production cost of the asphalt emulsifier of the invention is low, the process is simple, and no high-temperature reaction is required.

Description

technical field [0001] The invention relates to a carboxylic acid diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier and a preparation method thereof, belonging to the technical field of fine chemicals. Background technique [0002] Emulsified asphalt, especially cationic emulsified asphalt, is widely used in road construction and pavement maintenance because of its energy-saving and environmental protection, can improve construction conditions, and can effectively reduce excessive aging of asphalt and many other excellent application characteristics. [0003] The most critical factor affecting the road performance of emulsified asphalt is the asphalt emulsifier. At present, the main varieties of cationic asphalt emulsifiers at home and abroad include organic amines, quaternary ammonium salts, imidazolines, amides, etc., among which quaternary ammonium salt asphalt emulsifiers Agents include monoquaternary ammonium salts and diquaternary ammoniu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/14C07C303/32B01F17/06C08J3/03C08L95/00C09K23/06
CPCC07C227/02C07C303/32C07C309/14C08J3/03C08J2395/00C09K23/00
Inventor 施来顺于小梦马存飞
Owner SHANDONG UNIV
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