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Preparation method of phenolic emulsifier, emulsified bitumen and its application

A technology of emulsified asphalt and emulsifier, which is applied in the preparation of organic compounds, chemical instruments and methods, and the preparation of amino hydroxyl compounds. simple effect

Active Publication Date: 2012-06-27
JIANGSU SOBUTE NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Medworth Vaccine Company uses dodecylphenol to react with aminoethylpiperazine to synthesize a series of asphalt emulsifiers (US5019168, US4990591), but the cost of developing this emulsifier is relatively high, and the raw materials are not easy to obtain

Method used

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  • Preparation method of phenolic emulsifier, emulsified bitumen and its application
  • Preparation method of phenolic emulsifier, emulsified bitumen and its application
  • Preparation method of phenolic emulsifier, emulsified bitumen and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Get 10.13g (0.1mol) of diethylenetriamine and join in the reactor that 10ml of absolute ethanol and 15ml of dioxane are housed, slowly add 8.3g (0.1mol) of 37% formaldehyde solution after heating up to 10°C . React at 4 room temperature for 2h, then cool to 0°C to obtain an intermediate product, then add 20.6g (0.1mol) of octylphenol, raise the temperature to 80°C for 5h under reflux. The solvent was distilled off under reduced pressure to obtain a yellow viscous liquid, which was the final product, and the yield obtained by liquid chromatography was 90.2%. Save it for asphalt experiments.

[0037] The intermediate product was separated and purified by column 1 H-NMR and IR detection, the results are as follows:

[0038] 1 H-NMR (400MHz, CDCl 3 , δ, ppm): δ5.23(s, 2H), 2.81-2.60(m, 3*CH 2 , 6H), 2.4(m, 3H), 1.53(t, J=8.4Hz J=16.0, J=7.6Hz, 2H);

[0039] IR (neat): 3323cm -1 , 3213cm -1 , 1651cm -1 , 1180cm -1 , 1123cm -1 .

[0040] The final product is sepa...

Embodiment 2

[0049] Take 21.94g (0.15mol) of triethylenetetramine and add it into a reactor filled with 50ml of toluene, and slowly add 10.6g (0.1mol) of benzaldehyde solution after raising the temperature to 40°C. After reacting at 40°C for 5h, cool to 0°C to obtain an intermediate product, then add 23.4g (0.1mol) of decylphenol, raise the temperature to 120°C for 5h under reflux, and the yield obtained by liquid chromatography is 87.9% . The solvent was distilled off under reduced pressure to obtain a yellow viscous liquid, which was the final product, which was reserved for asphalt experiment.

[0050] The intermediate product was separated and purified by column 1 H-NMR and IR detection, the results are as follows:

[0051] 1 H-NMR (400MHz, CDCl 3 , δ, ppm) δ8.11(s, 1H), 7.62(d, J=7.6Hz, 2H), 7.29(t, J=7.6, J=15.6, J=8.0Hz, 3H), 3.67(t, J=15.2, J=7.6Hz, 2H), 2.85-2.57(m, 5*CH 2 , 10H), 2.35(m, 4H);

[0052] IR (neat): 3321cm -1 , 3217cm -1 , 1648cm -1 , 1596cm -1 , 1511cm -...

Embodiment 3

[0061] Take 17.5g (0.12mol) of triethylenetetramine and add it into a reactor filled with 50ml of water, and slowly add 12.45g of 37%-40% (0.15mol) formaldehyde solution after raising the temperature to 30°C. After reacting at 30°C for 2h, cool to 25°C to obtain an intermediate product, then add 26.2g (0.1mol) of dodecylphenol, then increase the temperature to 110°C for reflux reaction for 7h, the yield obtained by liquid chromatography was 96.5%. The solvent was distilled off under reduced pressure to obtain a yellow viscous liquid, which was the final product, which was reserved for asphalt experiment.

[0062] The intermediate product was separated and purified by column 1 H-NMR and IR detection, the results are as follows:

[0063] 1 H-NMR (400MHz, CDCl 3 , δ, ppm) δ5.32(s, 2H), 2.82-2.56(m, 5*CH 2 , 10H), 2.38(m, 4H), 1.53(t, J=7.6Hz J=14.8, J=7.2Hz, 2H);

[0064] IR (neat): 3321cm -1 , 3207cm -1 , 1644cm -1 , 1185cm -1 , 1118cm -1 .

[0065] The final product...

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Abstract

The invention relates to a preparation method of a phenolic emulsifier. The preparation method has advantages of simple synthesis technology, mild reaction condition and high yield, and is easy to realize industrialization. The invention also relates to emulsified bitumen emulsified by the phenolic emulsifier obtained by the above preparation method and an application thereof. The preparation method of the phenolic emulsifier contains the following steps of: performing a reaction between polyamines and aldehyde to generate aldimine, adding alkylphenol, performing a reaction to generate Mannich base, and acquiring the phenolic emulsifier, wherein the mol ratio of alkylphenol to aldehyde to polyamines is 1: (1-1.5): (1-1.5); alkylphenol is a compound as shown in the structural formula II; aldehyde is a compound as shown in the structural formula III; and polyamines is a compound as shown in the structural formula IV. The preparation method has advantages of simple synthesis technology, mild reaction condition and high yield, and is easy to realize industrialization. The emulsifier obtained by the preparation method has good emulsifying property. Each performance of the prepared emulsified bitumen meets the cationic emulsified bitumen standard and agitation performance technical indexes which are set by the Ministry of Communications.

Description

technical field [0001] The invention relates to a preparation method of a phenolic emulsifier, emulsified asphalt and application thereof. Background technique [0002] In recent years, my country's highway construction has developed rapidly. By the end of 2003, the total mileage of my country's highways had reached 1.81 million kilometers, including nearly 30,000 kilometers of expressways, ranking second in the world. By 2005, the national highway mileage will reach 1.95 million kilometers, including 34,000 kilometers of expressways. By 2010, the total mileage of my country's highways will reach 2.1 million to 2.3 million kilometers, and the "five vertical and seven horizontal" national highway trunk lines will be fully completed. It is estimated that by 2020, the total mileage of national highways will reach 2.6 million to 3 million kilometers, of which the total mileage of expressways will reach 70,000 kilometers, which requires a large amount of road construction funds....

Claims

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Application Information

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IPC IPC(8): C07C215/50C07C213/02C08J3/02C08L95/00C04B26/26
Inventor 缪昌文陈香刘加平洪锦祥刘至飞
Owner JIANGSU SOBUTE NEW MATERIALS
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