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A kind of preparation method of cationic gemini surfactant

A gemini surface and active agent technology is applied in the field of preparation of quaternary ammonium salt cationic gemini surfactants, which can solve problems such as adverse effects of industrialized production, corrosion of production equipment, difficulties in industrialization, etc., so as to facilitate industrialized operation and reduce equipment corrosion. , the effect of improving the reaction conversion rate

Active Publication Date: 2014-10-15
SHANGHAI FINE CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Acetone has a low boiling point and is highly volatile as a reaction solvent, which will adversely affect industrial production
[0007] To sum up, in these methods of preparing quaternary ammonium cationic gemini surfactants with epichlorohydrin as raw material, a large excess of epichlorohydrin or a large excess of tertiary amine is usually used as a raw material, which not only leads to waste of materials, but also must be separated and purified. Gemini surfactant products are obtained, and the subsequent separation and purification process is complicated and difficult; and epichlorohydrin is a toxic substance, if a large amount of residue will have a negative impact on the application of finished quaternary ammonium salt cationic gemini surfactants; in addition, the above Some of the methods need to react overnight, and the reaction cycle is long; when some prepare the tertiary amine hydrochloride intermediate, hydrogen chloride gas is passed into the tertiary amine, and the hydrogen chloride gas will cause great corrosion to the production equipment
Although the quaternary ammonium salt cationic gemini surfactant has excellent application performance, it is relatively difficult to industrialize due to its complicated preparation process.

Method used

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  • A kind of preparation method of cationic gemini surfactant
  • A kind of preparation method of cationic gemini surfactant
  • A kind of preparation method of cationic gemini surfactant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1: preparation 8-3 (OH)-8 ​​gemini cationic surfactant

[0048] The first step: in a 1000ml flask equipped with a mechanical stirring device and a condensing reflux tube, add 157g of octyldimethyl tertiary amine, and at room temperature, pass 221.2g of a hydrochloric acid solution with a mass concentration of 15% under stirring Add the dropping funnel into the flask for 20 minutes. After adding all the hydrochloric acid solution, continue stirring for 1 hour to obtain an aqueous solution of octyldimethyl tertiary amine hydrochloride intermediate (I).

[0049] Step 2: Add 93.5g of epichlorohydrin to 157g of octyldimethyl tertiary amine in a 500ml flask equipped with a mechanical stirring device and a condensing reflux tube, raise the temperature to 70°C, react for 2 hours, then add 1.5 g of triethanolamine was continued to react for 2 h to obtain a solution of octylglyceryl dimethyl ammonium chloride intermediate (II).

[0050] The third step: In a 2000ml fla...

Embodiment 2

[0054] Embodiment 2: preparation 12-3 (OH)-18 gemini cationic surfactant

[0055] The first step: in a 1000ml flask equipped with a mechanical stirring device and a condensing reflux tube, mix 213g of dodecyldimethyl tertiary amine with 213g of deionized water, and mix 121.7g of mass under stirring at room temperature The hydrochloric acid solution with a concentration of 30% is added to the mixture of dodecyldimethyl tertiary amine and water through the dropping funnel, and the addition time is 20min. After all the hydrochloric acid solution is added, continue stirring for 0.5h to obtain dodecyldimethyl tertiary amine Tertiary amine hydrochloride (I) aqueous solution.

[0056] Second step: in the 1000ml flask that has mechanical stirring device, condensing reflux tube is housed, the octadecyl dimethyl tertiary amine of 297.6g is dissolved in the isopropanol of 119g, adds 97.1g epichlorohydrin, The temperature was raised to 85°C, and after 3 hours of reaction, 15.7 g of triet...

Embodiment 3

[0061] Embodiment 3: preparation 18-3 (OH)-18 gemini cationic surfactant

[0062] The first step: in a 2000ml flask equipped with a mechanical stirring device and a condensing reflux tube, mix 297.6g of octadecyldimethyl tertiary amine with 372g of deionized water, and mix 111.1g of it under stirring at room temperature The hydrochloric acid solution with a mass concentration of 36.5% was added into the mixture of octadecyl dimethyl tertiary amine and deionized water through the dropping funnel, and the addition time was 20 minutes. After all the hydrochloric acid solution was added, the stirring was continued for 1 h to obtain octadecyl dimethylamine Methyl tertiary amine hydrochloride (I) aqueous solution.

[0063] The second step: in a 2000ml flask equipped with a mechanical stirring device and a condensing reflux tube, dissolve 297.6g of octadecyldimethyl tertiary amine in 297.5g of isopropanol, and add 101.8g of epichlorohydrin , the temperature was raised to 80°C, and a...

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Abstract

The invention belongs to the technical field of surfactants. The invention provides a method using epichlorohydrin and alkyl dimethyl tertiary amine (CH3-(CH2)n-N(CH3)2, n=7, 9, 11, 13, 15, 17) as raw materials, with 2 Preparation of a series of cationic gemini surfactants CH3(CH2)mN(CH3)2-CH2CH(OH)CH2-N(CH3)2(CH2)nCH3·Cl2 with -hydroxyl-1,3-propylene as linking group method. The method of the present invention overcomes the defect that a large excess of one material must be used to increase the reaction yield in the prior art, and the separation and purification step of the finished product can be omitted, the reaction cycle is short, the finished product has no epichlorohydrin residue, and is suitable for industrial scale production .

Description

technical field [0001] The invention belongs to the technical field of surfactants, in particular to a preparation method of a quaternary ammonium salt cationic gemini surfactant. Background technique [0002] As an important fine chemical, surfactant is widely used in various fields of production and life, and is known as "industrial monosodium glutamate". Surfactants have been rejuvenated, the varieties of surfactants are constantly improving, and the application fields are constantly expanding. They have become indispensable in high-tech fields such as material science, energy science, environmental science, life science and information science, and have become research hotspots. [0003] There are both hydrophilic and lipophilic parts in the molecular structure of surfactants, which can cause adsorption and enrichment on the surface or phase interface (liquid / liquid, liquid / solid), as well as self-assembly in the solution to form various organic compounds. Order combina...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01F17/18B01F17/38C07C213/04C07C215/40C09K23/18C09K23/38
Inventor 王丰收张威董万田杨庆利刘兵马丽娜余谱军张燕山李文迪
Owner SHANGHAI FINE CHEM CO LTD
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