CN102875393A - Synthetic method of hydroxyethyl dimethyl alkyl ammonium bromide - Google Patents
Synthetic method of hydroxyethyl dimethyl alkyl ammonium bromide Download PDFInfo
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- CN102875393A CN102875393A CN2012103470688A CN201210347068A CN102875393A CN 102875393 A CN102875393 A CN 102875393A CN 2012103470688 A CN2012103470688 A CN 2012103470688A CN 201210347068 A CN201210347068 A CN 201210347068A CN 102875393 A CN102875393 A CN 102875393A
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Abstract
The invention discloses a synthetic method of hydroxyethyl dimethyl alkyl ammonium bromide. The synthetic method comprises the following steps of: adding dimethyl hydroxyethyl amine and bromoalkane to a three-port flask according to a weight ratio of 0.8 to 1.5: l; transferring into a constant-temperature water bath pot at 60 DEG C for reacting; stopping agitating when a solution becomes a sticky state; stopping carrying out water bath; standing for a while to separate out white solid, namely a preliminary target product; dissolving the preliminary target product into acetone; naturally cooling and recrystallizing so as to separate out a thin white crystal at a common temperature; filtering, and repeating operations for two to three times; and drying obtained white crystal, namely a final target product. HDAB (hydroxyethyl dimethyl alkyl ammonium bromide) series products synthesized via the synthetic method disclosed by the invention has a good foaming property and very strong stability; and the foaming property is enhanced along with increase of a lipophilic group carbon chain, and foam tends towards a stable state.
Description
Technical field
The invention belongs to the organic chemical synthesis field, be specifically related to a kind of synthetic method of hydroxyethyl dimethyl alkyl brometo de amonio.
Background technology
Quaternary ammonium salt surface active agent can reduce surface tension effectively, have good wettability, wash the characteristics such as soil removability, higher biological safety, good heatproof stability by force, the quaternary surfactant that especially contains many alkyl more has many special performances.Many quaternary ammonium alkyl salt surfactant has the much higher surfactivity of more single alkane chain tensio-active agent, and has preferably bactericidal property.
Summary of the invention
The invention provides a kind of synthetic method of hydroxyethyl dimethyl alkyl brometo de amonio, take bromoalkane and dimethyl ethylol amine as raw material, synthesized a kind of quaternary ammonium salt surface active agent.
Be that 0.8～1.5:l joins in the there-necked flask with dimethyl ethylol amine and bromoalkane by molar ratio, the thermostat water bath of putting into 60 ℃ reacts, and stops when becoming sticky shape stirring; Close water-bath, place for some time, separate out white solid, be preliminary target product; Preliminary target product is dissolved in the acetone, and the naturally cooling recrystallization is separated out very thin white crystal at normal temperatures; Filter, repeat aforesaid operations 2～3 times, the white crystal that obtains is dry, be final target product.Be respectively hydroxyethyl dimethyl dodecyl bromination ammonium (HDAB-12), hydroxyethyl dimethyl Tetradecylammonium bromide (HDAB-l4) and hydroxyethyl dimethyl hexadecyl brometo de amonio (HDAB-16).
Preferred dimethyl ethylol amine and bromoalkane are l:l by molar ratio.
The synthetic HDAB series product of synthetic method of the present invention have good whipability, and very strong stability is also arranged, and along with the growth of oleophilic group carbochain, its whipability strengthens, and foam tends towards stability.
Embodiment
Below in conjunction with embodiment the synthetic method of hydroxyethyl dimethyl alkyl brometo de amonio of the present invention is described in detail; thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that protection scope of the present invention is made more explicit defining.
The raw material reagent that the present invention is used: bromoalkane, dimethyl ethylol amine, acetone, Silver Nitrate etc. are analytical pure.
Embodiment 1
Be that 0.8:l joins in the there-necked flask with dimethyl ethylol amine and bromoalkane by molar ratio, the thermostat water bath of putting into 60 ℃ reacts, and stops when becoming sticky shape stirring; Close water-bath, place for some time, separate out white solid, be preliminary target product; Preliminary target product is dissolved in the acetone, and the naturally cooling recrystallization is separated out very thin white crystal at normal temperatures; Filter, repeat aforesaid operations 2～3 times, the white crystal that obtains is dry, be final target product.Be respectively hydroxyethyl dimethyl dodecyl bromination ammonium (HDAB-12), hydroxyethyl dimethyl Tetradecylammonium bromide (HDAB-l4) and hydroxyethyl dimethyl hexadecyl brometo de amonio (HDAB-16).
Embodiment 2
Be that 1.5:l joins in the there-necked flask with dimethyl ethylol amine and bromoalkane by molar ratio, the thermostat water bath of putting into 60 ℃ reacts, and stops when becoming sticky shape stirring; Close water-bath, place for some time, separate out white solid, be preliminary target product; Preliminary target product is dissolved in the acetone, and the naturally cooling recrystallization is separated out very thin white crystal at normal temperatures; Filter, repeat aforesaid operations 2～3 times, the white crystal that obtains is dry, be final target product.Be respectively hydroxyethyl dimethyl dodecyl bromination ammonium (HDAB-12), hydroxyethyl dimethyl Tetradecylammonium bromide (HDAB-l4) and hydroxyethyl dimethyl hexadecyl brometo de amonio (HDAB-16).
Embodiment 3
Be that 1:l joins in the there-necked flask with dimethyl ethylol amine and bromoalkane by molar ratio, the thermostat water bath of putting into 60 ℃ reacts, and stops when becoming sticky shape stirring; Close water-bath, place for some time, separate out white solid, be preliminary target product; Preliminary target product is dissolved in the acetone, and the naturally cooling recrystallization is separated out very thin white crystal at normal temperatures; Filter, repeat aforesaid operations 2～3 times, the white crystal that obtains is dry, be final target product.Be respectively hydroxyethyl dimethyl dodecyl bromination ammonium (HDAB-12), hydroxyethyl dimethyl Tetradecylammonium bromide (HDAB-l4) and hydroxyethyl dimethyl hexadecyl brometo de amonio (HDAB-16).
The synthetic HDAB series product of synthetic method of the present invention have good whipability, and very strong stability is also arranged, and along with the growth of oleophilic group carbochain, its whipability strengthens, and foam tends towards stability.
Claims (2)
1. the synthetic method of a hydroxyethyl dimethyl alkyl brometo de amonio, it may further comprise the steps:
Be that 0.8～1.5:l joins in the there-necked flask with dimethyl ethylol amine and bromoalkane by molar ratio, the thermostat water bath of putting into 60 ℃ reacts, and stops when becoming sticky shape stirring; Close water-bath, place for some time, separate out white solid, be preliminary target product; Preliminary target product is dissolved in the acetone, and the naturally cooling recrystallization is separated out very thin white crystal at normal temperatures; Filter, repeat aforesaid operations 2～3 times, the white crystal that obtains is dry, be final target product.
2. the synthetic method of hydroxyethyl dimethyl alkyl brometo de amonio according to claim 1, it is characterized in that: described dimethyl ethylol amine and bromoalkane are 1:1 by molar ratio.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103470688A CN102875393A (en) | 2012-09-18 | 2012-09-18 | Synthetic method of hydroxyethyl dimethyl alkyl ammonium bromide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012103470688A CN102875393A (en) | 2012-09-18 | 2012-09-18 | Synthetic method of hydroxyethyl dimethyl alkyl ammonium bromide |
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| CN102875393A true CN102875393A (en) | 2013-01-16 |
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| CN2012103470688A Pending CN102875393A (en) | 2012-09-18 | 2012-09-18 | Synthetic method of hydroxyethyl dimethyl alkyl ammonium bromide |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0146097B1 (en) * | 1983-12-17 | 1988-06-08 | Hoechst Aktiengesellschaft | Oxyalkylated quaternary ammonium compounds, their preparation and their use as drag reducing agents |
| CN101381318A (en) * | 2008-10-22 | 2009-03-11 | 广州大学 | Microwave synthetic method of dodecyl methyl biethoxyl ammonium bromide |
-
2012
- 2012-09-18 CN CN2012103470688A patent/CN102875393A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0146097B1 (en) * | 1983-12-17 | 1988-06-08 | Hoechst Aktiengesellschaft | Oxyalkylated quaternary ammonium compounds, their preparation and their use as drag reducing agents |
| CN101381318A (en) * | 2008-10-22 | 2009-03-11 | 广州大学 | Microwave synthetic method of dodecyl methyl biethoxyl ammonium bromide |
Non-Patent Citations (5)
| Title |
|---|
| TINCA BURUIANA等: "Synthesis and Properties of Liquid Crystalline Urethane Methacrylates for Dental Composite Applications", 《JOURNAL OF POLYMER SCIENCE PART A: POLYMER CHEMISTRY》, vol. 49, 14 January 2011 (2011-01-14), pages 2622 - 2 * |
| WEI TONG等: "Critical Micellar Concentrations of Quaternary Ammonium Surfactants with Hydroxyethyl Substituents on Headgroups Determined by Isothermal Titration Calorimetry", 《J.CHEM.ENG.DATA》, vol. 55, 6 October 2010 (2010-10-06), pages 3766 - 2 * |
| XIAOMEI QIU等: "Enthalpies of Transfer of Amino Acids from Water to Aqueous Cationic Surfactants Solutions at 298.15 K", 《J.CHEM.ENG.DATA》, vol. 53, 22 March 2008 (2008-03-22), pages 942 * |
| 朱春光: "新型双子表面活性剂的合成及性能研究", 《精细石油化工进展》, vol. 12, no. 5, 31 May 2011 (2011-05-31) * |
| 赵田红等: "两性双子表面活性剂的合成及性能评价", 《应用化工》, vol. 40, no. 7, 31 July 2011 (2011-07-31) * |
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Application publication date: 20130116 |