Biquaternary ammonium salt type hydroxypropyl sodium phosphate asphalt emulsifier and preparation method thereof

A technology of sodium hydroxypropyl phosphate and asphalt emulsifier, applied in chemical instruments and methods, phosphorus organic compounds, organic chemistry, etc., can solve the problems of high requirements for production experimental equipment, high cost of emulsifier raw materials, and source restrictions, etc. Achieve excellent performance indicators, good aggregate adhesion and storage stability, and enhance the effect of charge strength

Inactive Publication Date: 2018-03-23
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-mentioned amphoteric asphalt emulsifiers and their preparation methods are: the cost of raw materials for the preparation of emulsifiers is high, the source is limited, high temperature reactions are required during preparation, and the requirements for production and experimental equipment are relatively high

Method used

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  • Biquaternary ammonium salt type hydroxypropyl sodium phosphate asphalt emulsifier and preparation method thereof
  • Biquaternary ammonium salt type hydroxypropyl sodium phosphate asphalt emulsifier and preparation method thereof
  • Biquaternary ammonium salt type hydroxypropyl sodium phosphate asphalt emulsifier and preparation method thereof

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preparation example Construction

[0051] For above asphalt emulsifier, the present invention also provides its preparation method, comprises the following steps:

[0052] (1) N-hydrogenated tallow-1,3-propylenediamine, alcohol solvent and propylene oxide are mixed and reacted to obtain reaction intermediate I, and the structural formula of said reaction intermediate I is

[0053]

[0054] Among them, n=1-3;

[0055] (2) Dissolve sodium dihydrogen phosphate in water, heat to a certain temperature, then gradually add epichlorohydrin, and mix and react to obtain reaction intermediate II, which is 3-chloro-2-hydroxypropyl phosphate sodium

[0056]

[0057] (3) Add the reaction intermediate II to the reaction intermediate I, and mix and react to obtain the diquaternary ammonium salt type sodium hydroxypropyl phosphate asphalt emulsifier;

[0058] Or, include the following steps:

[0059] (1) N-hydrogenated tallow-1,3-propylenediamine, alcohol solvent and propylene oxide are mixed and reacted to obtain reacti...

Embodiment 1

[0094] (1) Preparation of bisquaternary ammonium salt type sodium hydroxypropyl phosphate asphalt emulsifier (n=1):

[0095] 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 180.0g propylene oxide, and stir at 70°C for 3h.

[0096] 2) Add 491.4g sodium dihydrogen phosphate (NaH 2 PO 4 2H 2 O) and 966g of water, stir to dissolve, and heat to 85°C. Then 194.1 g of epichlorohydrin was added dropwise, and stirred at 85° C. for 7.5 h to obtain an aqueous solution of 3-chloro-2-hydroxypropyl phosphate sodium.

[0097] The above synthetic intermediate product was separated and purified by recrystallization and then detected by FTIR. The results are as follows: 3445cm -1 It is the stretching vibration absorption peak of O-H, 1635cm -1 C-O asymmetric stretching vibration absorption peak, 1297cm -1 It is the stretching vibration absorption peak of P=O, 1093cm -1 It is the stretchin...

Embodiment 2

[0107] (1) Preparation of bisquaternary ammonium salt type sodium hydroxypropyl phosphate asphalt emulsifier (n=2):

[0108] 1) Add 326.0g of N-hydrogenated tallow-1,3-propylenediamine and 330g of isopropanol into the reactor, heat and stir to dissolve. Then, 354.3 g of propylene oxide was gradually added, and the reaction was stirred at 70° C. for 3 h.

[0109] 2) Add 491.4g sodium dihydrogen phosphate (NaH 2 PO 4 2H 2 O) and 966g of water, stir to dissolve, and heat to 85°C. Then 194.1 g of epichlorohydrin was added dropwise, and stirred at 85° C. for 7.5 h to obtain an aqueous solution of 3-chloro-2-hydroxypropyl phosphate sodium.

[0110] 3) The aqueous solution of sodium 3-chloro-2-hydroxypropyl phosphate 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 diquaternary ammonium salt type sodium hydroxypropyl phosphate asphalt emulsifier was obtained, which was reserved for the emulsified asphalt tes...

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Abstract

The invention discloses a biquaternary ammonium salt type hydroxypropyl sodium phosphate asphalt emulsifier and a preparation method thereof. The asphalt emulsifier is prepared from the following rawmaterials in molar ratio: N-(hydrogenated tallow alkyl)trimethylenediamine, an alcohol solvent, propylene oxide, epichlorohydrin and sodium dihydrogen phosphate in a molar ratio of 1 mol:(5.00-11.00)mol:(3.00-9.20) mol:(2.00-2.30) mol:(3.00-3.45) mol. Alternatively, the asphalt emulsifier is prepared from N-(hydrogenated tallow alkyl)trimethylenediamine, the alcohol solvent, propylene oxide, epichlorohydrin, trisodium phosphate and hydrochloric acid in a molar ratio of 1 mol:(5.00-11.00) mol:(3.00-9.20) mol:(2.00-2.30) mol:(2.60-2.99) mol:(2.66-3.06)mol. The alcohol solvent is ethanol, methanol or isopropanol. The asphalt emulsifier has the advantages of easily available synthetic raw materials, low production cost and simple process, and does not need high-temperature reaction. Differenttypes of asphalt can be emulsified, the prepared emulsified asphalt is fine and uniform and has good storage stability, and cationic emulsified asphalt can be prepared.

Description

technical field [0001] The invention relates to a diquaternary ammonium salt type sodium hydroxypropyl phosphate asphalt emulsifier and a preparation method thereof, belonging to the technical field of fine chemicals. Background technique [0002] In road engineering, emulsified asphalt is suitable for asphalt pavement surface treatment, normal temperature asphalt mixture, as well as permeable layer, adhesive layer and sealing layer. It has the advantages of saving energy, prolonging the construction season, improving efficiency, improving construction conditions, and reducing environmental pollution. Asphalt emulsifiers are surfactants that can emulsify asphalt. There are many classification methods for asphalt emulsifiers. According to the type of ions, they mainly include anionic, cationic, nonionic and amphoteric. The amphoteric types are mainly betaine compounds, imidazoline compounds and amino acid compounds. [0003] However, the development of amphoteric asphalt emu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09C07F9/655C08J3/03C08L95/00
CPCC07F9/091C07F9/093C07F9/65505C08J3/03C08J2395/00C08L95/00
Inventor 施来顺巩雪笛于小梦马存飞
Owner SHANDONG UNIV
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