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Preparation method of 3- -(P-Nonyl)Phenoxy-2- Hydroxyproyl Trimethyl Ammonium Halide

A technology of hydroxypropyltrimethylammonium halide and nonylphenoxy, which is applied in the field of surfactant preparation, can solve problems that have not been reported, and achieve the effects of improving surface activity, easy production, and good control of reaction conditions

Inactive Publication Date: 2007-09-26
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of the important use of quaternary ammonium cationic surfactants, it is of great significance to research and develop new types of cationic surfactants. After searching, although there are hydroxypropyl groups embedded in the molecules of anionic surfactants AES and its surface The report that activity improves greatly, but inserts hydroxypropyl group in cationic surfactant molecule, synthesizes novel quaternary ammonium salt cationic surfactant containing benzene ring to reduce the cost of synthesis, but the method for improving surface activity has not been reported

Method used

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  • Preparation method of 3- -(P-Nonyl)Phenoxy-2- Hydroxyproyl Trimethyl Ammonium Halide
  • Preparation method of 3- -(P-Nonyl)Phenoxy-2- Hydroxyproyl Trimethyl Ammonium Halide

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Embodiment 1

[0036] The preparation method of 3-p-nonylphenoxy group-2-hydroxypropyltrimethylammonium halide comprises the steps:

[0037] (1) Synthesis of p-nonylphenyl glycidyl ether

[0038] Add 0.1 mol (about 22 g) of p-nonylphenol, 50 ml of toluene, and about 1 g of tetrabutylammonium bromide into a 250 ml four-neck flask and stir to dissolve; weigh 0.1 mol (4.0 g) of NaOH and dissolve in about 4 ml of distilled water Add it dropwise to a four-neck bottle, stir for 3 minutes and heat it with warm water. When the temperature rises to 50°C±1°C, add 0.2 moles of epichlorohydrin (about 16ml) dropwise, and finish adding in 15min to 16min, then raise the temperature to 70°C ℃±1℃, 5000 rpm vigorously stirred and reacted for 4h; after the reaction was completed, the product solution was slightly cooled and washed with 50℃ warm water in a separatory funnel for 2 to 3 times, then the upper organic phase was taken out and transferred to an Erlenmeyer flask , add 5 g of anhydrous sodium sulfate,...

Embodiment 2

[0044] The preparation method of 3-p-nonylphenoxy group-2-hydroxypropyltrimethylammonium halide comprises the steps:

[0045] (1) Synthesis of p-nonylphenyl glycidyl ether

[0046] Add p-nonylphenol, toluene, and tetrabutylammonium bromide into the four-necked bottle, stir to dissolve it; weigh NaOH, dissolve it in distilled water, drop it into the four-necked bottle, heat it with warm water after stirring for 2 minutes, when the temperature After rising to 50°C±1°C, add epichlorohydrin dropwise for 15min to 16min, then raise the temperature to 70°C±1°C, stir and react at 4000 rpm for 5h; after the reaction is completed, cool the product solution and use a 50°C Warm water was washed 3 times in a separatory funnel, then the upper organic phase was taken out, transferred to an Erlenmeyer flask, anhydrous sodium sulfate of 1 / 10 of the volume weight of the organic phase was added, and dried overnight; then the liquid was transferred to a pear-shaped flask, Distill toluene and epi...

Embodiment 3

[0054] The preparation method of 3-p-nonylphenoxy group-2-hydroxypropyltrimethylammonium halide comprises the steps:

[0055] (1) Synthesis of p-nonylphenyl glycidyl ether

[0056] Add p-nonylphenol, toluene, and tetrabutylammonium bromide into the four-necked bottle, stir to dissolve it; weigh NaOH, dissolve it in distilled water, drop it into the four-necked bottle, stir for 5 minutes, and heat it with warm water. After rising to 50°C±1°C, add epichlorohydrin dropwise, and finish adding in 15min~16min, then raise the temperature to 70°C±1°C, stir and react at 4500 rpm for 4.5h; Wash twice with warm water in a separatory funnel, then take out the upper organic phase, transfer it to an Erlenmeyer flask, add anhydrous sodium sulfate 1 / 9 of the volume weight of the organic phase, and dry it overnight; then transfer the liquid to a pear-shaped flask , use a rotary evaporator to distill toluene and epichlorohydrin to obtain colorless p-nonylphenyl glycidyl ether;

[0057] Wherei...

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Abstract

The invention discloses a making method of 3-p-nonylphenoxyacetic-2-hydroxypropyl trimethyl ammonium halides, which comprises the following steps: adopting toluene as catalyst and tetra butyl ammonium chloride as phase-transmitting catalyst in the alkaline condition to react p-nonyl phenol and epichlorohydrin at 70+-1 deg.c for 4-5h; obtaining p-nonylphenyl glycidic ester; dissolving p-nonylphenyl glycidic ester through 95%; adding trimethyl halogen acid at 40+-5 deg.c for 2h-3h; recrystallizing through acetic ester; obtaining the product; improving productivity obviously to purify the product.

Description

Technical field: [0001] The invention belongs to the field of preparation of surfactants in colloid and interface chemistry, in particular to a preparation method of a new quaternary ammonium salt cationic surfactant 3-p-nonylphenoxy-2-hydroxypropyltrimethylammonium halide . Background technique: [0002] It took 30 years from the successful development of cationic surfactants to mass production in the 1930s. It was not until the 1960s that people made great progress in the research on cationic surfactants. In the long-term development of cations, the main development direction is the research and application of nitrogen-containing cationic surfactants. Among them, there are many kinds of quaternary ammonium salt-type cationic surfactants, which are widely used and develop relatively rapidly. [0003] Quaternary ammonium salt-type cationic surfactants have important uses due to their adsorption on negatively charged surfaces and the formation of thin films on the surface. I...

Claims

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Application Information

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IPC IPC(8): C07C217/28C07C213/02C07C213/00
Inventor 尹宝霖魏西莲孙德志刘杰
Owner LIAOCHENG UNIV
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