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Phenol quaternary ammonium salt emulsifier and preparation method thereof

A technology of quaternary ammonium salts and emulsifiers, applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc., can solve problems such as pollution and large fuel consumption, and achieve simple process, good emulsification performance and high yield high effect

Active Publication Date: 2014-04-02
JIANGSU SOBUTE NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] During the use of road asphalt, in order to maintain the fluidity of the asphalt, a large amount of fuel will be consumed, and problems such as pollution will occur

Method used

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  • Phenol quaternary ammonium salt emulsifier and preparation method thereof
  • Phenol quaternary ammonium salt emulsifier and preparation method thereof
  • Phenol quaternary ammonium salt emulsifier and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 22g (0.1mol) of nonylphenol and add it to a reactor equipped with 30ml of pyridine and 16ml of water, and then add 9.2g (0.1mol) of epichlorohydrin. After reacting at 40°C for 3.5h, the intermediate product was obtained with a yield of 100%. Then 19.7g of 33% (0.11mol) trimethylamine solution was added, and the temperature was raised to 90°C for 5h. The product obtained by liquid chromatography The rate is 88.3%. The solvent was distilled off under reduced pressure to obtain a yellow viscous liquid, which was separated by a column to obtain the final product with a yield of 95.6%, which was reserved for asphalt experiment.

[0030] The intermediate product was separated and purified by column 1 H-NMR and IR detection, the results are as follows:

[0031] 1 H-NMR (400MHz, CDCl 3 , δppm) δ7.23(d, J=7.6, 2H), 6.75(d, J=7.6Hz, 2H), 4.12(d, J=8.4Hz, 2H), 4.08(m, 1H), 3.61(d , J=7.6Hz, 2H), 2.56(t, J=15.2Hz, J=7.6Hz, 2H), 2.21(s, 1H), 1.25-1.36(m, 14H), 0.96(t, J=8....

Embodiment 2

[0040] Take 22g (0.1mol) of nonylphenol and add it into a reactor containing 30ml of N,N-dimethylformamide, and then add 9.2g (0.1mol) of epichlorohydrin. After reacting at 20°C for 2h, the yield of the intermediate product was 100%, and then 13.2g (0.13mol) of triethylamine was added, and the temperature was raised to 80°C for 8h, and the yield obtained by liquid chromatography was 98.1%. . The solvent was distilled off under reduced pressure to obtain a yellow viscous liquid, which was separated by a column to obtain the final product with a yield of 79.1%, which was reserved for asphalt experiment.

[0041] The intermediate product was separated and purified by column 1 H-NMR and IR detection, the results are as follows:

[0042] 1 H-NMR (400MHz, CDCl 3 , δppm) δ7.23(d, J=7.6Hz, 2H), 6.75(d, J=7.6Hz, 2H), 4.12(d, J=8.4Hz, 2H), 4.08(m, 1H), 3.61( d, J=7.6Hz, 2H), 2.56(t, J=15.2Hz, J=7.6Hz, 2H), 2.21(s, 1H), 1.25-1.36(m, 14H), 0.96(t, J=8.4 Hz, J=16.0Hz, J=7.6Hz, 3H). ...

Embodiment 3

[0051] Take 22g (0.1mol) of nonylphenol and add it to a reactor equipped with 30ml of chloroform and 16ml of water, and then add 9.2g (0.1mol) of epichlorohydrin. After reacting at 30°C for 8h, the yield was 100% intermediate product, then 14.2g of 33% (0.15mol) methylamine solution was added, and the temperature was raised to 90°C for 6h, and the yield obtained by liquid chromatography was 90.5%. The solvent was distilled off under reduced pressure to obtain a yellow viscous liquid, which was separated by a column to obtain the final product with a yield of 88.2%, which was reserved for asphalt experiment.

[0052] The intermediate product was separated and purified by column 1 H-NMR and IR detection, the results are as follows:

[0053] 1 H-NMR (400MHz, CDCl 3 , δ, ppm) δ7.23(d, J=7.6Hz, 2H), 6.75(d, J=7.6Hz, 2H), 4.12(d, J=8.4Hz, 2H), 4.08(m, 1H), 3.61(d, J=7.6Hz, 2H), 2.56(t, J=15.2Hz, J=7.6Hz, 2H), 2.21(s, 1H), 1.25-1.36(m, 14H), 0.96(t, J =8.4Hz, J=16.0Hz, J=7.6Hz,...

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Abstract

The invention relates to a phenol quaternary ammonium salt emulsifier and a preparation method thereof. The preparation method has a simple process, mild reaction conditions and high yield, and is easy for realizing industrialization. The obtained phenol quaternary ammonium salt emulsifier can be used for effectively enhancing the stability and adhesion of emulsified asphalt. The preparation method of the phenol quaternary ammonium salt emulsifier comprises the following steps of: undergoing a ring-opening reaction on alkylphenol shown as a formula (II) and epoxy chloropropane to obtain an intermediate shown as a formula (III); and reacting the intermediate with amine shown as a structural formula (IV) to obtain the phenol quaternary ammonium salt emulsifier shown as a structural formula (I), wherein R1 is straight-chain alkyl with 8-14 carbon atoms; and R2=R3=R4=CH3, or R2=R3=R4=Et, or R2=R3=CH3 and R4=H, or R2=R3=H and R4=CH3, or R2=R3=Et and R4=H, or R2=R3=Buty and R4=H, or R2=R3=CH2CH2OH and R4=H.

Description

technical field [0001] The invention relates to a phenolic quaternary ammonium salt emulsifier and a preparation method thereof. Background technique [0002] Petroleum asphalt is an indispensable infrastructure material for transportation, construction and other industries. In the late 19th century, some developed countries in Europe and the United States began to use petroleum asphalt for road construction. At the beginning of the 20th century, petroleum asphalt was developed rapidly as a road construction material, with increasing varieties, increasing output, improving quality and widely used. It can be seen from the consumption of petroleum asphalt in various countries: asphalt used for roads accounts for 70% to 85% of the total consumption, industrial use accounts for 10% to 20%, and others only account for 2% to 4%. [0003] During the use of road asphalt, in order to maintain the fluidity of the asphalt, a large amount of fuel will be consumed, and problems such as...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/32C07C213/04B01F17/42C08J3/02C08L95/00C09K23/42
Inventor 缪昌文陈香洪锦祥周伟玲王文峰
Owner JIANGSU SOBUTE NEW MATERIALS