CN102701998A - Method for preparing quaternary ammonium salt foaming agent - Google Patents
Method for preparing quaternary ammonium salt foaming agent Download PDFInfo
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- CN102701998A CN102701998A CN2012101898817A CN201210189881A CN102701998A CN 102701998 A CN102701998 A CN 102701998A CN 2012101898817 A CN2012101898817 A CN 2012101898817A CN 201210189881 A CN201210189881 A CN 201210189881A CN 102701998 A CN102701998 A CN 102701998A
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- quaternary ammonium
- ammonium salt
- forming material
- pore forming
- preparation
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Abstract
The invention discloses a method for preparing a quaternary ammonium salt foaming agent and belongs to the field of chemical industry. The method for preparing the quaternary ammonium salt foaming agent comprises the following steps of: 1) adding tetramethylethylenediamine and bromotetradecane in a molar ratio of (1:2.0)-(1:2.5) into a reaction kettle; 2) adding solvent in an amount which is 20 to 70 percent based on the total weight of a reaction system; 3) adding a catalyst in an amount which is 0.3 to 0.8 percent based on the mass of bromotetradecane; and 4) stirring at the temperature of between 60 and 110 DEG C for 4 to 8 hours, and evaporating to obtain while solid, namely the quaternary ammonium salt foaming agent. The process for preparing the quaternary ammonium salt foaming agent is simple, efficient and economic and has obvious economic and social benefits; by the method, the quaternary ammonium salt foaming agent can be prepared quickly; and the foaming agent is excellent in performance.
Description
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 fields such as mineral of rare metals flotation, the mine displacement of reservoir oil.Common traditional cationic its staple of quaternary ammonium salt pore forming material is 12 (or 14,16) alkyl trimethyl ammonium; During preparation generally with water as solvent owing to there is gas to participate in reaction, need in the special equipment autoclave pressure, carry out; Reaction times reaches 20-30 hour, and power consumption is big.Add weight percent during use and surpass 1% cationic quaternary ammonium salt actives component, also need 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 the pore forming material superior performance possesses remarkable economical and social benefit.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of preparation method of quaternary ammonium salt pore forming material may further comprise the steps:
(1) in reaction kettle, 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 a reaction system gross weight;
(3) add catalyzer, catalyst consumption is the 0.3-0.8% of bromotetradecane quality;
(4) stir 4h ~ 8h down at 60 ~ 110 ℃, evaporating solvent obtains white solid, promptly described quaternary ammonium salt pore forming material.
Described solvent is a kind of in acetone, ethanol, Virahol, the n-propyl alcohol.
Described catalyzer is Soiodin or potassiumiodide.
The method of use of described quaternary ammonium salt pore forming material: in the aqueous solution to be foamed, add the quaternary ammonium salt pore forming material of its quality 0.05-0.1%, add the auxiliary agent of 0.5-1% again, half foam life period >=6 hour.
Described auxiliary agent is a coconut oil diethanol amide.
Beneficial effect of the present invention is:
(1) preparation technology of the present invention is simple, efficient, quick, economical, and the pore forming material superior performance possesses remarkable economical and social benefit.
(2) the present invention intends with ketone (acetone), alcohols (like ethanol, Virahol, n-propyl alcohol etc.) etc. as reaction solvent; Through suitable raising temperature of reaction; Auxiliary with a little catalyzer, make the reactive behavior of one of raw material halohydrocarbon improve, thereby shorten the reaction times significantly.
When (3) using; Owing to have two hydrophobic alkane chains that lean on very closely, use amount seldom just can reach very high surfactivity on the cationic quaternary ammonium salt pore forming material molecular structure of the present invention's preparation, have very strong latherability; Foamy body is high during foaming, has good stability.
Embodiment
A kind of preparation method of quaternary ammonium salt pore forming material may further comprise the steps:
(1) in reaction kettle, 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 a reaction system gross weight;
(3) add catalyzer, catalyst consumption is the 0.3-0.8% of bromotetradecane quality;
(4) stir 4h ~ 8h down at 60 ~ 110 ℃, evaporating solvent obtains white solid, promptly described quaternary ammonium salt pore forming material.
Described solvent is a kind of in acetone, ethanol, Virahol, the n-propyl alcohol.
Described catalyzer is Soiodin or potassiumiodide.
The method of use of described quaternary ammonium salt pore forming material: in the aqueous solution to be foamed, add the quaternary ammonium salt pore forming material of its quality 0.05-0.1%, add the auxiliary agent of 0.5-1% again, half foam life period >=6 hour.
Described auxiliary agent is a coconut oil diethanol amide.
Reaction formula:
Embodiment 1
Bromotetradecane 8.94 g (0.0322mol), Tetramethyl Ethylene Diamine 1.50g (0.0129mol) and the anhydrous n-propyl alcohol of 3ml are joined in the 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 at first vacuum distilling is taken off most solvent n-propyl alcohol, and productive rate is 91%.
Embodiment 2
Bromotetradecane 8.22 g (0.0297mol) Tetramethyl Ethylene Diamine 1.50g (0.0129mol) and 5ml Virahol are joined in the 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 at first vacuum distilling is taken off most solvent Virahol, and productive rate is 86%.
Embodiment 3
Bromotetradecane 8.22 g (0.0297mol) Tetramethyl Ethylene Diamine 1.50g (0.0129mol) and 3ml ethanol are joined in the 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 at first vacuum distilling is taken off most etoh solvent, and productive rate is 82%.
Use prescription (weight percentage):
Cationic quaternary ammonium salt actives 0.05%-0.1%,
Coconut oil diethanol amide 0.5-1%
Method of use:
Join by the formulation weight percentage composition and to treat in the blistered solution stirring and dissolving.
The above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to covering scope of the present invention.
Claims (5)
1. the preparation method of a quaternary ammonium salt pore forming material, it is characterized in that: described preparation method may further comprise the steps:
(1) in reaction kettle, 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 a reaction system gross weight;
(3) add catalyzer, catalyst consumption is the 0.3-0.8% of bromotetradecane quality;
(4) stir 4h ~ 8h down at 60 ~ 110 ℃, evaporating solvent obtains white solid, promptly described quaternary ammonium salt pore forming material.
2. the preparation method of quaternary ammonium salt pore forming material according to claim 1 is characterized in that: described solvent is a kind of in acetone, ethanol, Virahol, the n-propyl alcohol.
3. the preparation method of quaternary ammonium salt pore forming material according to claim 1 is characterized in that: described catalyzer is Soiodin or potassiumiodide.
4. the preparation method of quaternary ammonium salt pore forming material according to claim 1; It is characterized in that: the method for use of described quaternary ammonium salt pore forming material: the quaternary ammonium salt pore forming material that in the aqueous solution to be foamed, adds its quality 0.05-0.1%; The auxiliary agent that adds 0.5-1% again, half foam life period >=6 hour.
5. the preparation method of quaternary ammonium salt pore forming material according to claim 4 is characterized in that: described auxiliary agent is a coconut oil diethanol amide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210189881.7A CN102701998B (en) | 2012-06-11 | 2012-06-11 | Method for preparing quaternary ammonium salt foaming agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210189881.7A CN102701998B (en) | 2012-06-11 | 2012-06-11 | Method for preparing quaternary ammonium salt foaming agent |
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| Publication Number | Publication Date |
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| CN102701998A true CN102701998A (en) | 2012-10-03 |
| CN102701998B CN102701998B (en) | 2014-05-21 |
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| CN201210189881.7A Expired - Fee Related CN102701998B (en) | 2012-06-11 | 2012-06-11 | Method for preparing quaternary ammonium salt foaming agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106674018A (en) * | 2015-11-06 | 2017-05-17 | 中国石油化工股份有限公司 | Method for synthesizing asymmetrical biquaternary ammonium salt and application of method |
| CN106674017A (en) * | 2015-11-06 | 2017-05-17 | 中国石油化工股份有限公司 | Preparation method and use of asymmetric bis-quaternary ammonium salt |
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| CN101607183A (en) * | 2008-06-20 | 2009-12-23 | 中国科学院成都有机化学有限公司 | Carboxylic acid betaine type gemini surfactant and preparation method |
| US7683035B1 (en) * | 1999-02-23 | 2010-03-23 | Qiagen, Gmbh | Method of stabilizing and/or isolating nucleic acids |
| CN101717221A (en) * | 2009-11-24 | 2010-06-02 | 中国矿业大学(北京) | Foaming agent for soil engineering |
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2012
- 2012-06-11 CN CN201210189881.7A patent/CN102701998B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US7683035B1 (en) * | 1999-02-23 | 2010-03-23 | Qiagen, Gmbh | Method of stabilizing and/or isolating nucleic acids |
| CN101607183A (en) * | 2008-06-20 | 2009-12-23 | 中国科学院成都有机化学有限公司 | Carboxylic acid betaine type gemini surfactant and preparation method |
| CN101717221A (en) * | 2009-11-24 | 2010-06-02 | 中国矿业大学(北京) | Foaming agent for soil engineering |
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| CHUNWEI GUO等: "Integrating statistical and experimental protocols to model and design novel Gemini surfactants with promising critical micelle concentration and low environmental risk", 《CHEMOSPHERE》 * |
| M. EL ACHOURI等: "Synthesis of some cationic gemini surfactants and their inhibitive e.ect on iron corrosion in hydrochloric acid medium", 《CORROSION SCIENCE》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106674018A (en) * | 2015-11-06 | 2017-05-17 | 中国石油化工股份有限公司 | Method for synthesizing asymmetrical biquaternary ammonium salt and application of method |
| CN106674017A (en) * | 2015-11-06 | 2017-05-17 | 中国石油化工股份有限公司 | Preparation method and use of asymmetric bis-quaternary ammonium salt |
| CN106674017B (en) * | 2015-11-06 | 2018-12-28 | 中国石油化工股份有限公司 | A kind of synthetic method and its application of asymmetry bi-quaternary ammonium salt |
| CN106674018B (en) * | 2015-11-06 | 2018-12-28 | 中国石油化工股份有限公司 | A kind of method and its application synthesizing asymmetric bi-quaternary ammonium salt |
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| CN102701998B (en) | 2014-05-21 |
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