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Preparation method and separation method of surfactant containing amino terminal and diamine group

The technology of a surfactant and a separation method, which is applied in the field of preparation of surfactants, can solve the problems of cumbersome preparation process, difficult separation process, complicated separation operation, etc., and achieves the effects of simple operation process, saving human resources, and simple operation process.

Active Publication Date: 2015-11-18
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the development of medical science and technology and the enhancement of human awareness of environmental protection, this type of surfactant has a broad application prospect. However, due to the cumbersome and long-term preparation process of this type of surfactant, the separation process is difficult, and the equipment and equipment required for separation It is more expensive, the separation operation is complicated, and the exchange resin used in the conventional separation inevitably occurs between the exchange resin and the product, resulting in product loss and low separation efficiency. (Fu Haiyan, Zeng Guangming, Yuan Xingzhong, Huang Guo, Shi Jingang, Zhong Hua. Journal of Biology, 2003, Volume 20, Issue 6, Pages 1-4.) and the literature "Application and Development Trend of Biosurfactants" ( Yang Shidi. "Application and Development Trend of Biosurfactants", Today's Science and Technology, 2002, Volume 9, 40-41.) and other articles have summarized these difficulties as the main problems hindering the wide application of this type of surfactants. It can be seen that , Reducing the difficulty of preparation, separation and purification is the core content of this type of surfactant research field. The present invention is just to solve the above problems, thereby providing a simple, economical and efficient preparation, separation and purification with biological safety The method of the surfactant containing amino terminal and diamine group

Method used

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  • Preparation method and separation method of surfactant containing amino terminal and diamine group
  • Preparation method and separation method of surfactant containing amino terminal and diamine group
  • Preparation method and separation method of surfactant containing amino terminal and diamine group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The route of preparing the tensio-active agent containing amino terminal and diamine group by octadecanoic acid is:

[0033]

[0034] Add octadecanoic acid solid and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide solid and 1-hydroxybenzotriazole solid in the round bottom flask, then add dichloromethane to dissolve, Stir evenly at room temperature to obtain a mixed solution; slowly drop the mixed solution into 1,2-(2-aminoethoxy)ethane through a constant-pressure dropping funnel, and carry out a stirring reaction under an ice-salt bath (can be obtained through a high-efficiency Thin-layer chromatography silica gel plate to monitor the reaction), after the reaction is completed, pour the obtained reaction solution into saturated saline, at this time, a white jelly-like small molecule gel is precipitated; the dichloromethane in the white jelly-like small molecule gel is filtered and water to obtain a white solid, which is a mixture of amino-terminated and diamine-based s...

Embodiment 2

[0046] The preparation of a mixture of surfactants containing amino-terminal and diamine groups is basically the same as in Example 1, except that octadecanoic acid is replaced by hexadecanoic acid to obtain a mixture of surfactants containing amino-terminal and diamine groups.

[0047] When the mixture is added dropwise to 1,2-(2-aminoethoxy)ethane, hexadecanoic acid solid: 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide solid : When the molar ratio of 1-hydroxybenzotriazole solid: 1,2-(2-aminoethoxy)ethane is 1:1:1:4, the surface activity of the amino-terminal and diamine-containing In the mixture of agents, the surfactant containing amino terminal accounts for 90-95% of the mass of the mixture, and the surfactant containing diamine groups accounts for 5-10% of the mass of the mixture.

[0048] When the mixture is added dropwise to 1,2-(2-aminoethoxy)ethane, hexadecanoic acid solid: 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide solid : When the molar ratio of 1-hydroxybenzotr...

Embodiment 3

[0053] The preparation of the mixture of surfactants containing amino-terminal and diamine groups is basically the same as in Example 1, except that octadecanoic acid is replaced by myristic acid to obtain a mixture of surfactants containing amino-terminal and diamine groups.

[0054] When the mixture is added dropwise to 1,2-(2-aminoethoxy)ethane, among which myristic acid solid: 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide solid : When the molar ratio of 1-hydroxybenzotriazole solid: 1,2-(2-aminoethoxy)ethane is 1:1:1:4, the surface activity of the amino-terminal and diamine-containing In the mixture of agents, the surfactant containing amino terminal accounts for 90-92% of the mass of the mixture, and the surfactant containing diamine groups accounts for 8-10% of the mass of the mixture.

[0055] When the mixture is added dropwise to 1,2-(2-aminoethoxy)ethane, among which myristic acid solid: 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide solid : When the molar ratio of 1-...

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Abstract

The invention relates to a method for preparing and separating surfactants which have high biological safety and contain amino terminal and diamino. The method comprises the following steps: adding fatty acid solids, 1-(3-dimethylaminopropyl)-3-vinyl carbodiimide solid and 1-hydroxybenzotriazole solids into dichloromethane, and dissolving to obtain a mixed solution; dropwise adding the mixed solution into 1,2-(2-aminoethoxy) ethane, reacting in an ice-salt bath, pouring the obtained reaction solution into saturated salt water, and performing suction filtration on the separated jelly-shaped small molecule gel, thus obtaining a mixture of the surfactants containing amino terminal and diamino; and adding the obtained mixture into a chromatographic column filled with silica gel, eluting by using gradient mixed eluant of dichloromethane and methanol, and separating the mixture of the surfactants containing the amino terminal and diamino, thus respectively obtaining a surfactant containing the amino terminal and a surfactant containing the diamino.

Description

technical field [0001] The invention relates to the preparation and separation of surfactants, in particular to the preparation and separation methods of surfactants containing amino terminal and diamine groups with biological safety. Background technique [0002] Surfactants have the functions and functions of emulsification, dispersion, solubilization, flocculation, and decontamination. These functions have been applied and played an important role in many industrial fields such as detergent, textile, papermaking, leather processing, pigment paint, printing, medicine, food fermentation and petrochemical industry. Therefore, the research and development of the preparation, separation and purification of novel surfactants has important theoretical significance and application value. Among them, surfactants containing amino terminal and diamine groups have received extensive attention from researchers at home and abroad (Aleksandar Todorovic, Jerry Ryan Holder, Rayna M. Bauz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/18C07C231/02B01F17/46C09K23/46
Inventor 江龙马雪盛仲瀚
Owner INST OF CHEM CHINESE ACAD OF SCI
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