CN102701998B

CN102701998B - A kind of preparation method of quaternary ammonium salt foaming agent

Info

Publication number: CN102701998B
Application number: CN201210189881.7A
Authority: CN
Inventors: 赵剑曦; 游毅; 刘小斌
Original assignee: Fuzhou University
Current assignee: Fuzhou University
Priority date: 2012-06-11
Filing date: 2012-06-11
Publication date: 2014-05-21
Anticipated expiration: 2032-06-11
Also published as: CN102701998A

Abstract

本发明公开了一种季铵盐起泡剂的制备方法，属于化工领域。该制备方法包括以下步骤：（1）在反应釜中加入四甲基乙二胺和溴代十四烷，两者的摩尔比为1:2.0~1:2.5；（2）加入溶剂，溶剂用量为反应体系总重量的20%~70%；（3）加入催化剂，催化剂的用量为溴代十四烷质量的0.3-0.8％；（4）在60~110℃下搅拌4h~8h，蒸发溶剂得到白色固体，即所述的季铵盐起泡剂。本发明的制备工艺简单、高效、快速、经济，起泡剂性能优越，具备显著的经济和社会效益。The invention discloses a preparation method of a quaternary ammonium salt foaming agent, which belongs to the field of chemical industry. The preparation method comprises the following steps: (1) adding tetramethylethylenediamine and tetradecane bromide into a reaction kettle, the molar ratio of the two is 1:2.0~1:2.5; (2) adding a solvent, the amount of solvent 20%~70% of the total weight of the reaction system; (3) Add catalyst, the amount of catalyst is 0.3-0.8% of the mass of tetradecane bromide; (4) Stir at 60~110°C for 4h~8h, evaporate the solvent Obtain white solid, namely described quaternary ammonium salt foaming agent. The preparation process of the invention is simple, efficient, fast and economical, the foaming agent has superior performance, and has remarkable economic and social benefits.

Description

A kind of preparation method of quaternary ammonium salt pore forming material

Technical field

The invention belongs to chemical field, be specifically related to a kind of preparation method of quaternary ammonium salt pore forming material.

Background technology

Cationic quaternary ammonium salt pore forming material is widely used in the field such as mineral of rare metals flotation, the mine displacement of reservoir oil.Common traditional cationic its main component of quaternary ammonium salt pore forming material is 12 (or 14,16) alkyl trimethyl ammonium, when preparation, generally using water as solvent, owing to there being gas to participate in reaction, need in special equipment autoclave pressure, carry out, reaction times reaches 20-30 hour, and power consumption is large.When use, add weight percent to exceed 1% cationic quaternary ammonium salt actives component, also need to add many kinds of auxiliary agents simultaneously, synergy, use cost is high.

Summary of the invention

The object of the present invention is to provide a kind of preparation method of quaternary ammonium salt pore forming material, preparation technology of the present invention is simple, efficient, quick, economical, and pore forming material superior performance possesses significant economic and social benefit.

For achieving the above object, the present invention adopts following technical scheme:

A kind of preparation method of quaternary ammonium salt pore forming material comprises the following steps:

(1) in reactor, add Tetramethyl Ethylene Diamine and bromotetradecane, both mol ratios are 1:2.0 ~ 1:2.5;

(2) add solvent, solvent load is 20% ~ 70% of reaction system gross weight;

(3) add catalyzer, the consumption of catalyzer is the 0.3-0.8% of bromotetradecane quality;

(4) at 60 ~ 110 ℃, stir 4h ~ 8h, evaporating solvent obtains white solid, i.e. described quaternary ammonium salt pore forming material.

Described solvent is the one in acetone, ethanol, Virahol, n-propyl alcohol.

Described catalyzer is sodium iodide or potassiumiodide.

The using method of described quaternary ammonium salt pore forming material: add the quaternary ammonium salt pore forming material of its quality 0.05-0.1% in the aqueous solution to be foamed, then add the auxiliary agent of 0.5-1%, half foam life period >=6 hour.

Described auxiliary agent is coconut oil diethanol amide.

Beneficial effect of the present invention is:

(1) preparation technology of the present invention is simple, efficient, quick, economical, and pore forming material superior performance possesses significant economic and social benefit.

(2) the present invention intends using ketone (acetone), alcohols (as ethanol, Virahol, n-propyl alcohol etc.) etc. as reaction solvent, by suitable raising temperature of reaction, auxiliary with a little catalyzer, the reactive behavior of one of raw material halohydrocarbon is improved, thus Reaction time shorten significantly.

(3) while use, on cationic quaternary ammonium salt pore forming material molecular structure prepared by the present invention, owing to thering are two hydrophobic alkane chains that lean on very closely, use little amount just can reach very high surfactivity, there is very strong latherability, when foaming, foamy body is high, has good stability.

Embodiment

(2) add solvent, solvent load is 20% ~ 70% of reaction system gross weight;

Described solvent is the one in acetone, ethanol, Virahol, n-propyl alcohol.

Described catalyzer is sodium iodide or potassiumiodide.

Described auxiliary agent is coconut oil diethanol amide.

Reaction formula:

。

Embodiment 1

By bromotetradecane 8.94 g(0.0322mol), Tetramethyl Ethylene Diamine 1.50g(0.0129mol) and the anhydrous n-propyl alcohol of 3ml join in 50mL there-necked flask, add 0.8% catalyzer and stirrer and load onto prolong, be warming up to 100 ℃, back flow reaction 8 hours.Reaction product is the de-solvent n-propyl alcohol to the greatest extent of vacuum distilling first, and productive rate is 91%.

Embodiment 2

By bromotetradecane 8.22 g(0.0297mol) Tetramethyl Ethylene Diamine 1.50g(0.0129mol) and 5ml Virahol join in 50mL there-necked flask, add 0.6% catalyzer and stirrer and load onto prolong, be warming up to 84 ℃, back flow reaction 8 hours.Reaction product is the de-solvent Virahol to the greatest extent of vacuum distilling first, and productive rate is 86%.

Embodiment 3

By bromotetradecane 8.22 g(0.0297mol) Tetramethyl Ethylene Diamine 1.50g(0.0129mol) and 3ml ethanol join in 50mL there-necked flask, add 0.8% catalyzer and stirrer and load onto prolong, be warming up to 80 ℃, back flow reaction 8 hours.Reaction product is the de-etoh solvent to the greatest extent of vacuum distilling first, and productive rate is 82%.

Use formula (weight percentage):

Cationic quaternary ammonium salt actives 0.05%-0.1%,

Coconut oil diethanol amide 0.5-1%

Using method:

Join in solution to be bubbled stirring and dissolving by formulation weight percentage composition.

The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.

Claims

1. a preparation method of quaternary ammonium salt foaming agent, is characterized in that: described preparation method comprises the following steps:

(1) Add tetramethylethylenediamine and tetradecane bromide into the reaction kettle, the molar ratio of the two is 1:2.0~1:2.5;

(2) Add solvent, the amount of solvent is 20%~70% of the total weight of the reaction system;

(3) Adding a catalyst, the amount of the catalyst is 0.6-0.8% of the mass of tetradecane bromide;

(4) Stir at 100°C for 4h~8h, evaporate the solvent to obtain a white solid, which is the quaternary ammonium salt foaming agent;

Described solvent is the one in Virahol, n-Propanol;

Described catalyst is sodium iodide or potassium iodide;

The method of using the quaternary ammonium salt foaming agent: add 0.05-0.1% of the quality of the quaternary ammonium salt foaming agent to the aqueous solution to be foamed, and then add 0.5-1% of the auxiliary agent, and the half-life of the foam is ≥ 6 hours ;

The auxiliary agent is coconut oil diethanolamide.