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A kind of primary amide 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 fields of sulfonate preparation, cyanide reaction preparation, chemical instruments and methods, etc. It can solve the problems of high temperature reaction, high cost, source limitation, etc., and achieve system stability , Improve stability, enhance the effect of charge intensity

Inactive Publication Date: 2019-02-26
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that the preparation steps are cumbersome, the cost is high, and high temperature reaction is required
[0006] 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
[0009] 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 primary amide diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier and its preparation method
  • A kind of primary amide diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier and its preparation method
  • A kind of primary amide 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 primary amide diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier is provided, comprising the steps:

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

[0052]

[0053] (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 (i.e. sodium 3-chloro-2-hydroxypropyl sulfonate);

[0054] (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 the primary amide bisquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emu...

Embodiment 1

[0063] (1) Preparation of primary amide diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier:

[0064] 1) Add 326.0g of N-hydrogenated tallow-1,3-propylenediamine and 330g of isopropanol into the reactor, heat and stir to dissolve. Then, 216.8 g of acrylamide was gradually added, and the reaction was stirred at 70° C. for 3 h.

[0065] The above synthetic intermediate product was separated and purified by recrystallization and then detected by FTIR. The results are as follows: 3440cm -1 and 3369cm -1 O-H stretching vibration absorption peak at 3190cm -1 The N-H stretching vibration absorption peak at 2916cm -1 and 2850cm -1 The asymmetric and symmetric stretching vibration absorption peaks of methylene respectively, 1669cm -1 It is the amide group C=O stretching vibration absorption peak, 1471cm -1 For the asymmetric bending vibration of methylene, 1409cm -1 Asymmetric bending vibration of the methyl group at 1261cm -1 and 1076cm -1 C-N st...

Embodiment 2

[0079] (1) Preparation of primary amide diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier:

[0080] 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, 216.8 g of acrylamide was gradually added, and the reaction was stirred at 70° C. for 3 h.

[0081] 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.

[0082] 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. The primary amide diquaternary ammonium salt type sodium hydroxypropyl sulfonate asphalt emulsifier was obtained, which was reserved for the emulsifie...

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Abstract

The invention discloses a primary amide biquaternary ammonium salt type hydroxypropyl sodium sulfonate asphalt emulsifier, the molecular structure of which is as shown in the specification. The primary amide biquaternary ammonium salt type hydroxypropyl sodium sulfonate asphalt emulsifier is prepared from the raw materials including N-hydrogenated tallow-1,3-diaminopropane, an alcohols solvent, acrylamide, epoxy chloropropane and sodium bisulfate at the molar ratio of (5.00-11.00) mol: (3.00-3.10) mol: (2.00-2.30) mol: (2.10-2.50) mol. The invention has the following advantages: production cost of the asphalt emulsifier is low; the process is simple; and high-temperature reaction is not required.

Description

technical field [0001] The invention relates to a primary amide 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] Asphalt emulsifier is an amphiphilic molecule with hydrophobic and hydrophilic groups. Asphalt emulsifier plays a decisive role in the production and application of emulsified asphalt. It is not only related to the preparation and storage stability of emulsified asphalt. It also directly determines important indicators such as the breaking speed and setting time of emulsified asphalt. [0003] Asphalt emulsifiers are divided into cationic and anionic emulsifiers according to the different ionic charge properties. Among them, the development of cationic asphalt emulsifiers is relatively late, but in practical applications, it is found that cationic asphalt emulsifiers have better interactions with various mineral mater...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/03C08L95/00C07C303/32C07C309/14
CPCC07C227/02C07C303/32C07C309/14C08J3/03C08J2395/00C08L95/00C08L2201/54C07C229/16C07C309/08
Inventor 施来顺于小梦马存飞
Owner SHANDONG UNIV
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