Preparation method of trimeric surfactant

Abstract

The invention discloses a preparation method of a trimeric surfactant, and belongs to the technical field of surfactant preparation, the method comprises the following steps: mixing chloroacetyl chloride and tris (2-aminoethyl) amine, reacting to obtain trichloro acetylated tris (2-aminoethyl) amine, reacting the obtained trichloro acetylated tris (2-aminoethyl) amine with N, N-dimethyl formamide, and reacting to obtain the trimeric surfactant. And reacting with N, N-dimethyl dodecylamine to obtain the trimeric surfactant. When the prepared trimeric surfactant is used in an industrial cleaning agent, the use amount of the surfactant in the industrial cleaning agent is greatly reduced, the COD value of the industrial cleaning agent is greatly reduced, the environmental protection treatment cost of industrial cleaning waste liquid is greatly reduced, the preparation process is simple, the reaction condition is mild, the reaction period is short, and the method is suitable for industrial production. The raw materials are low in cost and simple in source, and the obtained product is high in purity and easy for industrial production.

Description

Technical Field

[0001] The invention belongs to the technical field of surfactant preparation, and in particular relates to a method for preparing a trimerized surfactant. Background Art

[0003] Two or more amphiphilic moieties are chemically bonded on or near their head groups through linking groups to obtain dimers (usually called Gemini surfactants), trimers, tetramers, or even oligomeric surfactants with higher oligomerization. Oligomeric surfactants have many properties superior to traditional single-chain surfactants, such as lower critical micelle concentration (CMC), higher surface activity, lower Krafft point, excellent rheological properties, novel and diverse aggregate structures, and better wetting effects, etc. They show stronger capabilities in washing, sterilization, emulsification, dispersion, and antiseptic properties.

[0004] Therefore, it is necessary to develop a new type of high-efficiency surfactant with higher surface activity, higher assembly ability at the gas-liquid interface, solid surface and solution phase, which can integrate the properties of emulsification degreasing, decontamination, metal corrosion inhibition, antibacterial, bactericidal and low foaming at extremely low concentrations as the main agent of industrial cleaning agents. Summary of the invention

[0005] In order to solve the problems in the prior art, the present invention provides a method for preparing a trimerized surfactant, comprising the following steps: mixing chloroacetyl chloride and tris(2-aminoethyl)amine to obtain trichloroacetylated tris(2-aminoethyl)amine, and reacting the obtained trichloroacetylated tris(2-aminoethyl)amine with N,N-dimethyldodecylamine to obtain the trimerized surfactant.

[0006] Preferably, it is characterized in that the molar ratio of the chloroacetyl chloride to tris(2-aminoethyl)amine is 1:3-7, and the molar ratio of the trichloroacetylated tris(2-aminoethyl)amine to N,N-dimethyldodecylamine is 1:2-5.

[0007] Preferably, the mixed reaction step of chloroacetyl chloride and tris(2-aminoethyl)amine is: slowly adding tris(2-aminoethyl)amine to chloroacetyl chloride within 1-2 hours at room temperature, then heating to 40-45° C. to react for 6-7 hours, and after the reaction is completed, oil-water separation is performed to obtain trichloroacetylated tris(2-aminoethyl)amine.

[0008] Preferably, the reaction step of trichloroacetylated tris(2-aminoethyl)amine and N,N-dimethyldodecylamine is: uniformly mixing trichloroacetylated tris(2-aminoethyl)amine and N,N-dimethyldodecylamine, adding them to a solvent, reacting them at a temperature of 60-70° C. for 12-15 hours, evaporating the obtained product to remove the solvent, and then recrystallizing and vacuum drying to obtain the trimerized surfactant.

[0009] Preferably, the solvent is methanol with a concentration of 20%.

[0010] Preferably, the additive for recrystallization is ethanol.

[0011] Compared with the prior art, the present invention has the following advantages: The trimerized surfactant prepared by the present invention has higher surface activity and stronger aggregation ability. It can form large aggregates through strong hydrophobic association between molecules at extremely low concentrations, greatly improving the use efficiency of the surfactant. It can integrate the performances of emulsification degreasing, decontamination, metal corrosion inhibition, antibacterial, sterilization, low foaming, etc. at extremely low concentrations. When used in industrial cleaning agents, the amount of surfactant used in the industrial cleaning agent is greatly reduced, the COD value of the industrial cleaning agent is greatly reduced, and the environmental protection treatment cost of industrial cleaning waste liquid is greatly reduced. The preparation process involved in the present invention is simple, the reaction conditions are mild, the reaction cycle is short, the raw material cost is low and the source is simple, the obtained product has high purity, and is easy to industrialize. DETAILED DESCRIPTION

[0012] The technical scheme of the present invention will be further described in detail below in conjunction with specific embodiments. It should be understood that the following embodiments are only exemplary descriptions and explanations of the present invention, and should not be construed as limiting the scope of protection of the present invention. All technologies realized based on the above content of the present invention are included in the scope that the present invention is intended to protect.

[0013] Unless otherwise specified, the raw materials and reagents used in the following examples are commercially available or can be prepared by known methods. Example

[0014] A method for preparing a trimerized surfactant comprises the following steps: 1) Slowly add tri(2-aminoethyl)amine to chloroacetyl chloride at room temperature within 1-2 hours, the molar ratio of chloroacetyl chloride to tri(2-aminoethyl)amine is 1:3-7, then heat to 40-45°C for reaction for 6-7 hours, and after the reaction is completed, separate the oil and water to obtain trichloroacetylated tri(2-aminoethyl)amine; 2) Trichloroacetylated tris(2-aminoethyl)amine and N,N-dimethyldodecylamine are uniformly mixed, added into a solvent methanol, the molar ratio of trichloroacetylated tris(2-aminoethyl)amine to N,N-dimethyldodecylamine is 1:2-5, reacted at a temperature of 60-70° C. for 12-15 hours, the obtained product is evaporated to remove the solvent, and then recrystallized through ethanol and vacuum dried to obtain the trimerized surfactant. Example

[0015] A method for preparing a trimerized surfactant comprises the following steps: 1) Slowly add tri(2-aminoethyl)amine to chloroacetyl chloride at room temperature within 1 hour, the molar ratio of chloroacetyl chloride to tri(2-aminoethyl)amine is 1:3, then heat to 40°C for 6 hours, and separate the oil and water after the reaction is completed to obtain trichloroacetylated tri(2-aminoethyl)amine; 2) Trichloroacetylated tris(2-aminoethyl)amine and N,N-dimethyldodecylamine are uniformly mixed, added into a solvent methanol, the molar ratio of trichloroacetylated tris(2-aminoethyl)amine to N,N-dimethyldodecylamine is 1:2-5, reacted at a temperature of 60-70° C. for 12-15 hours, the obtained product is evaporated to remove the solvent, and then recrystallized through ethanol and vacuum dried to obtain the trimerized surfactant. Example

[0016] A method for preparing a trimerized surfactant comprises the following steps: 1) Slowly add tri(2-aminoethyl)amine to chloroacetyl chloride at room temperature within 1-2 hours, the molar ratio of chloroacetyl chloride to tri(2-aminoethyl)amine is 1:3-7, then heat to 40-45°C for reaction for 6-7 hours, and after the reaction is completed, separate the oil and water to obtain trichloroacetylated tri(2-aminoethyl)amine; 2) Trichloroacetylated tris(2-aminoethyl)amine and N,N-dimethyldodecylamine are uniformly mixed, added into a solvent methanol, the molar ratio of trichloroacetylated tris(2-aminoethyl)amine to N,N-dimethyldodecylamine is 1:2-5, reacted at a temperature of 60-70° C. for 12-15 hours, the obtained product is evaporated to remove the solvent, and then recrystallized through ethanol and vacuum dried to obtain the trimerized surfactant. Example

[0017] A method for preparing a trimerized surfactant comprises the following steps: 1) Slowly add tri(2-aminoethyl)amine to chloroacetyl chloride at room temperature within 1-2 hours, the molar ratio of chloroacetyl chloride to tri(2-aminoethyl)amine is 1:3-7, then heat to 40-45°C for reaction for 6-7 hours, and after the reaction is completed, separate the oil and water to obtain trichloroacetylated tri(2-aminoethyl)amine; 2) Trichloroacetylated tris(2-aminoethyl)amine and N,N-dimethyldodecylamine are uniformly mixed, added into a solvent methanol, the molar ratio of trichloroacetylated tris(2-aminoethyl)amine to N,N-dimethyldodecylamine is 1:2-5, reacted at a temperature of 60-70° C. for 12-15 hours, the obtained product is evaporated to remove the solvent, and then recrystallized through ethanol and vacuum dried to obtain the trimerized surfactant.

[0018] The emulsifying properties of the trimerized surfactants prepared in Examples 1-4 were determined by the water separation time method. -2 mol / L is 1059-1128s, while the emulsification capacity of DTAB is 735s. Its emulsification performance is significantly better than that of DTAB. This is because its molecules are arranged more closely on the air / water interface than DTAB, the interfacial film strength is increased, and the emulsion stability is enhanced.

[0019] The corrosion inhibition performance of the trimerized surfactant prepared in Examples 1-4 was determined by weight loss method. Under the condition of 1 mol / L hydrochloric acid as the acidic medium, the corrosion inhibition efficiency of the trimerized surfactant for N80 steel increased with the increase of solution solubility. When the surfactant concentration was 5.9×10 -4 mol / L, the corrosion inhibition efficiency is ≥92.36%, indicating that it has a good corrosion inhibition effect in strong acid solution.

[0020] The carbon, hydrogen and nitrogen content of the trimer surfactant prepared in Examples 1-4 was analyzed by elemental analysis. The results showed that the theoretical values ​​of the carbon, hydrogen and nitrogen content were very close to the measured values, and the purity was ≥96.3%.

[0021] The trimerized surfactant prepared in Examples 1-4 is prepared into an industrial cleaning agent, the original ingredients of which include: 25% alkylphenol polyoxyethylene ether, 6% propylene glycol methyl ether, 6% polyacrylic acid, 10% aminotriacetic acid, 7% auxiliary agent, and 46% deionized water.

[0022] After the trimer surfactant is added, the ingredients include: 25% of alkylphenol polyoxyethylene ether, 0.1% of trimer surfactant, 6% of polyacrylic acid, 10% of aminotriacetic acid, 7% of auxiliary agent, and 51.9% of deionized water.

[0023] The prepared industrial cleaning agent was tested and the results were as follows:

[0024] The above results show that the trimerized surfactant prepared by the present invention improves the utilization efficiency of the surfactant, greatly reduces the amount of the surfactant in the industrial cleaning agent when added to the industrial cleaning agent, greatly reduces the COD value of the industrial cleaning agent, and greatly reduces the cost of environmental protection treatment of industrial cleaning waste liquid.

[0025] The above descriptions are merely embodiments of the present invention. It should be pointed out that, for those skilled in the art, various changes, modifications, substitutions and variations can be made to these embodiments without departing from the technical principles of the present invention. These changes, modifications, substitutions and variations should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing a trimerized surfactant, characterized in that: The method comprises the following steps: mixing chloroacetyl chloride and tri(2-aminoethyl)amine to obtain trichloroacetylated tri(2-aminoethyl)amine, and reacting the obtained trichloroacetylated tri(2-aminoethyl)amine with N,N-dimethyldodecylamine to obtain the trimerized surfactant.

2. The method for preparing a trimerization surfactant according to claim 1, characterized in that: The molar ratio of the chloroacetyl chloride to tris(2-aminoethyl)amine is 1:3-7, and the molar ratio of the trichloroacetylated tris(2-aminoethyl)amine to N,N-dimethyldodecylamine is 1:2-5.

3. The method for preparing a trimerization surfactant according to claim 1, characterized in that: The mixed reaction step of chloroacetyl chloride and tri(2-aminoethyl)amine is as follows: tri(2-aminoethyl)amine is slowly added into chloroacetyl chloride within 1-2 hours at room temperature, then heated to 40-45° C. for reaction for 6-7 hours, and after the reaction is completed, oil-water separation is performed to obtain trichloroacetylated tri(2-aminoethyl)amine.

4. The method for preparing a trimerization surfactant according to claim 1, characterized in that: The reaction steps of trichloroacetylated tris(2-aminoethyl)amine and N,N-dimethyldodecylamine are as follows: uniformly mixing trichloroacetylated tris(2-aminoethyl)amine and N,N-dimethyldodecylamine, adding them into a solvent, reacting them at a temperature of 60-70° C. for 12-15 hours, evaporating the obtained product to remove the solvent, and then recrystallizing and vacuum drying to obtain the trimerized surfactant.

5. The method for preparing a trimerized surfactant according to claim 4, characterized in that: The solvent is methanol with a concentration of 20%.

6. The method for preparing a trimerized surfactant according to claim 4, characterized in that: The additive for the recrystallization is ethanol.

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