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

AI Technical Summary

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

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

Examples

Experimental program
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Example Embodiment

[0035] Example 1

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

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

[0038] Add 0.1 mol (about 22g) of p-nonylphenol, 50ml of toluene, and about 1g of tetrabutylammonium bromide into a 250ml four-necked flask and stir to dissolve it; weigh out 0.1mol (4.0g) of NaOH and dissolve in about 4ml of distilled water Into a four-necked flask, stir for 3 minutes and then heat with warm water. When the temperature rises to 50℃±1℃, add 0.2 mol (about 16ml) of epichlorohydrin dropwise, add it in 15min to 16min, and then heat up to 70 ℃±1℃, 5,000 rpm, vigorously stir the reaction for 4 hours; after the reaction is completed, the product solution is slightly cooled and washed with 50 ℃ warm water in a separatory funnel for 2 to 3 times, then the upper organic phase is taken out and transferred to a conical flask , Add 5g of anhydrous sodium sulfate and dry overnight; th...

Example Embodiment

[0043] Example 2

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

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

[0046] Add p-nonylphenol, toluene, and tetrabutylammonium bromide into a four-necked flask, stir to dissolve it; weigh out NaOH, dissolve it in distilled water, drop it into the four-necked flask, stir for 2min and then heat with warm water. After the temperature is raised to 50℃±1℃, add epichlorohydrin dropwise, 15min~16min complete, then heat up to 70℃±1℃, stir for 5h at 4000 rpm; after the reaction, cool the product solution and use 50℃ Wash 3 times with warm water in a separatory funnel, then take out the upper organic phase, transfer to a conical flask, add anhydrous sodium sulfate of 1 / 10 of the volume weight of the organic phase, and dry overnight; then transfer the liquid to a pear-shaped flask, Use a rotary evaporator to distill toluene and epichlorohydrin to obtain colorless p-n...

Example Embodiment

[0053] Example 3

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

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

[0056] Add p-nonylphenol, toluene, and tetrabutylammonium bromide into a four-neck flask, stir to dissolve it; weigh out NaOH, dissolve it in distilled water, drop it into the four-neck flask, stir for 5 minutes and then heat it with warm water. After raising to 50℃±1℃, add epichlorohydrin dropwise, 15min~16min after adding, then heat to 70℃±1℃, stirring at 4500 rpm for 4.5h; after the reaction is completed, the product solution is cooled and used at 50℃ Wash the upper organic phase in a separatory funnel twice, then take out the upper organic phase, transfer to a conical flask, add anhydrous sodium sulfate of 1 / 9 of the volume weight of the organic phase, and dry overnight; then transfer the liquid to a pear-shaped flask , Use a rotary evaporator to distill toluene and epichlorohydrin to...

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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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