十二烷基硫酸鈉表面活性劑制備及性能研究

1、實驗七 十二烷基硫酸鈉表面活性劑的制備及性能研究一、實驗目的1、了解表面活性劑的基本性質及應用2、學習表面活性劑的分離純化技術3、學習表面活性劑性質的測試方法二、實驗背景十二烷基硫酸鈉, 別名為月桂醇硫酸鈉, 是陰離子硫酸酯類表面活性劑的典型代表, 由于它具有良好的乳化性、起泡性、可生物降解、耐堿及耐硬水等特點, 廣泛應用于化工、紡織、印染、制藥、造紙、石油、化妝品和洗滌用品制造等各種工業(yè)部門。表面活性劑的開發(fā)與應用已成為一個非常重要的行業(yè)，通過本綜合實驗讓學生掌握表面活性劑研究的最基本實驗技術和知識。三、儀器和藥品儀器：三口燒瓶，攪拌裝置，分液漏斗，旋轉蒸發(fā)器，抽濾裝置，容量瓶（50mL），

2、紅外光譜分析儀，核磁共振，表面張力測定儀。藥品：正十二醇，氨基磺酸，尿素，濃硫酸，無水乙醇，氫氧化鈉，乙醚，氯化鈉，重蒸餾水。四、實驗提示1、查閱文獻資料，依據實驗室提供的條件，設計制備十二烷基硫酸鈉的實驗方案。2、提出產物鑒定方法。3、提出測定表面活性劑表面張力、臨界膠束濃度的方法。4、寫出研究報告。五、思考題1、采用氨基磺酸進行磺化反應的優(yōu)點是什么？2、鹽的加入對表面張力及臨界膠束濃度有什么影響？六、參考文獻1、陳敏，崔慶飛，氨基磺酸法合成十二烷基硫酸鈉綜合實驗. 實驗技術與管理，2007,24(4):35-37.2、陳聯群, 李春蘭, 葉蓮, 等. 十二烷基硫酸鈉的提純與純度測定. 內江

3、師范學院學報, 2005, 20(6): 35-37.3、Alissa J. Prosser, Elias I. Franses, New thermodynamic/electrostatic models of adsorption and tension equilibria of aqueous ionic surfactant mixtures: application to sodium dodecyl sulfate/sodium dodecyl sulfonate systems, Journal of Colloid and Interface Science, 2003,

4、263: 606-615The synthesize and properties study of sodium dodecyl sulfateThe experiment purposes1 / 41、Understanding the basic properties and application of surfactant2、Study the technology of isolation and purification for surfactant3、Study the measuremenst of surfactant propertiesBackgroundSodium

5、dodecyl sulfate, SDS, other names for laurel sulfate, is a common type of anionic surfactant. It has excellent emulsifying, foaming property, biodegradability, good alkaline resistance, and hard water instance, etc. SDS is widely used in non-phosphorus washing powder, liquid detergents and home wash

6、ing products, textile, printing and dyeing industry, petrochemical products, and industrial hard surface cleaning agents, etc. SDS is widely used in many fields such as chemical industry, textile, dyeing, pharmaceutical, paper making, oil field, detergent, cosmetic, personal hygiene aid industries a

7、nd fields. Developing and application of surfactant has become an important field. The purpose of the comprehensive experiment is to Understanding the basic experiment technology and knowledge.Instruments and reagentsInstruments and apparatus: three-necked flask, agitator, pressure funnel，separalory

8、 funnel, rotary evaporator, filtration apparatus, volumetric flask (50mL), FT-IR spectrometer, NMR equipment, surface tension meter.Reagents: dodecanol, aminosulfonic acid, urea, sulfuric acid, anhydrous alcohol, sodium hydroxide, ethyl ether, Sodium chloride, distilled water.The notice of experimen

9、t1、Consulting literature material and based on the Condition provided by laboratory, design the scheme of preparing SDS2、Proposes appraisal method of the product3、Proposes measurement methods for surface tension, critical micelle concentration4、Provide the thesis.Question1、What is the advantages of

10、the sulfonation reaction used aminosulfonic acid as sulfonation reagent?2、What is the effects of salt on surface tension and critical micelle concentration?Reference1、Chen M. Cui Q. F. The syntheses experiment of synthesis of sodium dodecyl sulfate from aminosulfonic acid, Experimental Technology an

11、d Management, 2007, 24(4): 35-37.2、Chen L. Q. Li C. L. Ye L. Zeng P. Zhu Y. P. Purification and purity determination of sodium dodecyl sulfate, Journal of Neijiang Teachers College, 2005, 20(6): 35-37.3、Alissa J. Prosser, Elias I. Franses, New thermodynamic/electrostatic models of adsorption and ten

12、sion equilibria of aqueous ionic surfactant mixtures: application to sodium dodecyl sulfate/sodium dodecyl sulfonate systems, Journal of Colloid and Interface Science, 2003, 263: 606-615合成步驟1、向配有攪拌裝置的三口燒瓶中加入含40 mL正十二醇（過量部分起稀釋作用），混合均勻的9.7g氨基磺酸和2.4g尿素，再滴加少量濃硫酸，在105110 oC下攪拌反應70 min，用30%的NaOH溶液處理，放盡NH3后倒出即得到粗產品。2、在粗產物中加入120 mL水，加熱使產物呈流態(tài)并將其倒出，用少量乙醚洗滌后，濃縮冷卻結晶，即可得到產物。過量的十二醇溶于乙醚，可以回收干燥后再利用。或者：將第1步反應后的混合液轉移入分流漏斗中，用乙醚萃取3