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CN106117090B - The Asymmetric Gemini surfactants of sulfonic group containing carboxyl and its microwave preparation - Google Patents

The Asymmetric Gemini surfactants of sulfonic group containing carboxyl and its microwave preparation Download PDF

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CN106117090B
CN106117090B CN201610429668.7A CN201610429668A CN106117090B CN 106117090 B CN106117090 B CN 106117090B CN 201610429668 A CN201610429668 A CN 201610429668A CN 106117090 B CN106117090 B CN 106117090B
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acid diester
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carboxyl
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maleic acid
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CN106117090A (en
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吕斌
王泓棣
马建中
苏娇娇
翟蕊
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
    • C07C303/22—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C309/00—Sulfonic acids; Halides, esters, or anhydrides thereof
    • C07C309/01—Sulfonic acids
    • C07C309/02—Sulfonic acids having sulfo groups bound to acyclic carbon atoms
    • C07C309/03—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
    • C07C309/17—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing carboxyl groups bound to the carbon skeleton
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Abstract

本发明涉及含羧基‑磺酸基不对称Gemini表面活性剂及其微波制备方法。运用微波水热法合成表面活性剂的研究鲜有报道。本发明利用脂肪酸单乙醇酰胺马来酸双酯、十二烷基磺基琥珀酸酯二钠盐和亚硫酸氢钠制得脂肪酸单乙醇酰胺磺基琥珀酸双酯，滴加氯乙酸溶液，转入高通量微波消解/萃取/合成工作站反应，中和，得到一种含羧基—磺酸基不对称Gemini表面活性剂。本发明基于价廉易得的天然脂肪酸为原料，采用微波法制备的含羧基‑磺酸基不对称Gemini表面活性剂避免了传统油浴加热反应时间长、反应条件苛刻、反应中原料易升华、原料和产物易发生氧化反应、产品色泽较差等缺点，具有良好的市场应用性。The invention relates to an asymmetric Gemini surfactant containing a carboxyl-sulfonic acid group and a microwave preparation method thereof. There are few reports on the synthesis of surfactants by microwave hydrothermal method. The present invention utilizes fatty acid monoethanolamide maleic acid diester, dodecyl sulfosuccinate disodium salt and sodium bisulfite to prepare fatty acid monoethanolamide sulfosuccinic acid diester, drips chloroacetic acid solution, and transfers Put it into a high-throughput microwave digestion/extraction/synthesis workstation for reaction and neutralization to obtain a carboxyl-sulfonic acid group-containing asymmetric Gemini surfactant. The present invention is based on cheap and easy-to-obtain natural fatty acids as raw materials, and the carboxyl-sulfonic acid group-containing asymmetric Gemini surfactant prepared by microwave method avoids the traditional oil bath heating reaction time is long, the reaction conditions are harsh, and the raw materials are easy to sublime during the reaction. The raw materials and products are prone to oxidation reactions, and the product has poor color, etc., and has good market applicability.

Description

含羧基-磺酸基不对称Gemini表面活性剂及其微波制备方法Asymmetric Gemini surfactant containing carboxyl-sulfonic acid group and microwave preparation method thereof

技术领域technical field

本发明涉及一种表面活性剂，具体涉及一种含羧基-磺酸基不对称Gemini表面活性剂及其微波制备方法。The invention relates to a surfactant, in particular to a carboxyl-sulfonic acid group-containing asymmetric Gemini surfactant and a microwave preparation method thereof.

背景技术Background technique

随着科学技术、工业生产和多学科跨领域的不断发展，表面活性剂的应用范围会越来越广，会关联到生产生活等众多方面，随着绿色化学理念和人们环保意识增强，表面活性剂也被赋予更高的性能要求。此时，Gemini表面活性剂应运而生，Gemini表面活性剂由于其独特的结构、良好的生物降解性、优良的表面活性成为相关工作者的研究重点。磺酸盐型Gemini表面活性剂是一种非常重要的阴离子型Gemini表面活性剂，其具有高表面活性、很好的水溶性、润湿性、分散性、耐酸碱性也得到很大提高，所以磺酸盐型Gemini表面活性剂将会在多个领域得到应用。With the continuous development of science and technology, industrial production and multidisciplinary cross-fields, the scope of application of surfactants will become wider and wider, and will be related to many aspects of production and life. Agents are also given higher performance requirements. At this time, Gemini surfactant came into being, and Gemini surfactant has become the research focus of relevant workers because of its unique structure, good biodegradability, and excellent surface activity. Sulfonate Gemini surfactant is a very important anionic Gemini surfactant, which has high surface activity, good water solubility, wettability, dispersibility, and acid and alkali resistance have also been greatly improved. So sulfonate Gemini surfactant will be applied in many fields.

微波是一种普遍存在的超高频电磁波。现如今，微波技术已经引进化工领域40多年，近年来，在众多合成方法中，微波水热法已逐渐脱颖而出。与传统方法相比，微波合成法具有热能利用率高、条件温和、加热速度快以及均匀、非热微波效应等优点。因此，微波水热法越来越受到人们的关注。然而运用微波水热法合成表面活性剂的研究并不多见。Microwave is a ubiquitous ultra-high frequency electromagnetic wave. Nowadays, microwave technology has been introduced into the chemical industry for more than 40 years. In recent years, among many synthetic methods, microwave hydrothermal method has gradually come to the fore. Compared with the traditional method, the microwave synthesis method has the advantages of high thermal energy utilization rate, mild conditions, fast heating speed and uniform, non-thermal microwave effect. Therefore, microwave hydrothermal method has attracted more and more attention. However, there are few studies on the synthesis of surfactants by microwave hydrothermal method.

发明内容Contents of the invention

本发明的目的是提供一种含羧基-磺酸基不对称Gemini表面活性剂及其微波制备方法。The object of the present invention is to provide a kind of asymmetric Gemini surfactant containing carboxyl-sulfonic acid group and microwave preparation method thereof.

本发明所采用的技术方案为：The technical scheme adopted in the present invention is:

含羧基-磺酸基不对称Gemini表面活性剂的微波制备方法，其特征在于：The microwave preparation method containing carboxyl-sulfonic acid group asymmetric Gemini surfactant is characterized in that:

由以下步骤实现：Achieved by the following steps:

步骤一：制备脂肪酸单乙醇酰胺磺基琥珀酸双酯：Step 1: Preparation of fatty acid monoethanolamide sulfosuccinic acid diester:

称取9.3-10.8质量份的脂肪酸单乙醇酰胺马来酸双酯，加入三口烧瓶中，用质量分数为40%的氢氧化钠溶液将其pH中和至7，加入3.1-4.3质量份十二烷基磺基琥珀酸酯二钠盐；Weigh 9.3-10.8 parts by mass of fatty acid monoethanolamide maleic acid diester, add it to a three-necked flask, neutralize its pH to 7 with a sodium hydroxide solution with a mass fraction of 40%, and add 3.1-4.3 parts by mass of twelve Alkyl sulfosuccinate disodium salt;

称取2.2-2.4质量份的亚硫酸氢钠，并且将其配成30%的亚硫酸氢钠溶液滴加到三口烧瓶中，在70-80℃的水浴锅中使体系搅拌均匀；将反应物转入微波消解仪中在温度140℃-180℃、功率600W的条件下反应40-90min得到脂肪酸单乙醇酰胺磺基琥珀酸双酯；Weigh 2.2-2.4 parts by mass of sodium bisulfite, and make 30% sodium bisulfite solution dropwise into a three-necked flask, and stir the system evenly in a water bath at 70-80°C; Transfer to a microwave digestion apparatus and react for 40-90min at a temperature of 140°C-180°C and a power of 600W to obtain fatty acid monoethanolamide sulfosuccinic acid diester;

步骤二：制备含羧基-磺酸基不对称Gemini表面活性剂：Step 2: Preparation of asymmetric Gemini surfactants containing carboxyl-sulfonic acid groups:

称取3.4-4.2质量份的氯乙酸，配成30%溶液，并将其溶液用氢氧化钠调节pH至7；Weigh 3.4-4.2 parts by mass of chloroacetic acid to make a 30% solution, and adjust the pH of the solution to 7 with sodium hydroxide;

将氯乙酸溶液滴加至18.36-22.44质量份的肪酸单乙醇酰胺磺基琥珀酸双酯后，调节体系pH至7，搅拌均匀；After adding the chloroacetic acid solution dropwise to 18.36-22.44 parts by mass of fatty acid monoethanolamide sulfosuccinic acid diester, adjust the pH of the system to 7, and stir evenly;

将反应物转入高通量微波消解/萃取/合成工作站控制温度70-90℃，功率600w，反应90-120min，每间隔20min测其pH并调节至7，得到一种含羧基—磺酸基不对称Gemini表面活性剂。Transfer the reactant to a high-throughput microwave digestion/extraction/synthesis workstation, control the temperature at 70-90°C, power 600w, react for 90-120min, measure the pH every 20min and adjust it to 7 to obtain a carboxyl-sulfonic acid group-containing Asymmetric Gemini Surfactants.

步骤一中，脂肪酸单乙醇酰胺马来酸双酯选自十二酸单乙醇酰胺马来酸双酯、油酸单乙醇酰胺马来酸双酯、硬脂酸单乙醇酰胺马来酸双酯、菜籽油单乙醇酰胺马来酸双酯。In step one, fatty acid monoethanolamide maleic acid diester is selected from dodecanoic acid monoethanolamide maleic acid diester, oleic acid monoethanolamide maleic acid diester, stearic acid monoethanolamide maleic acid diester, Rapeseed oil monoethanolamide maleate diester.

如所述的含羧基-磺酸基不对称Gemini表面活性剂的微波制备方法制得的表面活性剂。The surfactant prepared by the microwave preparation method of the carboxyl-sulfonic acid group-containing asymmetric Gemini surfactant.

本发明具有以下优点：The present invention has the following advantages:

本发明利用高通量微波消解/萃取/合成工作站采用微波法在脂肪酸单乙醇酰胺马来酸双酯上，引入亲水基团羧基与磺酸基，制得含羧基-磺酸基不对称Gemini表面活性剂中间体，磺化率可以达到85%，叔胺化产率可达80%。本方法避免了传统油浴加热反应时间长、反应条件苛刻、反应中原料易升华、原料和产物易发生氧化反应、产品色泽较差等缺点，具有良好的市场应用性。The invention utilizes a high-throughput microwave digestion/extraction/synthesis workstation to introduce a hydrophilic group carboxyl group and a sulfonic acid group into a fatty acid monoethanolamide maleic acid diester by using a microwave method to obtain a carboxyl-sulfonic acid group-containing asymmetric Gemini Surfactant intermediates, the sulfonation rate can reach 85%, and the tertiary amination yield can reach 80%. The method avoids the disadvantages of traditional oil bath heating, such as long reaction time, harsh reaction conditions, easy sublimation of raw materials in the reaction, easy oxidation reaction of raw materials and products, and poor color of products, and has good market applicability.

具体实施方式detailed description

下面结合具体实施方式对本发明进行详细的说明。The present invention will be described in detail below in combination with specific embodiments.

本发明利用微波水热法，以十二酸单乙醇酰胺与马来酸单酯为原料，制备得表面活性剂中间体十二酸单乙醇酰胺马来酸双酯，并对双酯进行磺化、叔胺化，引入亲水基团，制备得一种性能良好的含羧基-磺酸基不对称Gemini表面活性剂。The present invention utilizes the microwave hydrothermal method to prepare the surfactant intermediate dodecanoic acid monoethanolamide maleic acid diester by using dodecanoic acid monoethanolamide and maleic acid monoester as raw materials, and sulfonates the diester , tertiary amination, and the introduction of hydrophilic groups to prepare a carboxyl-sulfonic acid group-containing asymmetric Gemini surfactant with good performance.

本发明利用高通量微波消解/萃取/合成工作站采用微波法在脂肪酸单乙醇酰胺马来酸双酯上，引入亲水基团羧基与磺酸基，其反应方程式为：The present invention uses a high-throughput microwave digestion/extraction/synthesis workstation to introduce a hydrophilic group carboxyl group and a sulfonic acid group on the fatty acid monoethanolamide maleic acid diester using a microwave method, and the reaction equation is:

具体由以下步骤实现：Specifically, it is realized by the following steps:

步骤一：制备脂肪酸单乙醇酰胺磺基琥珀酸双酯：Step 1: Preparation of fatty acid monoethanolamide sulfosuccinic acid diester:

称取9.3-10.8质量份的脂肪酸单乙醇酰胺马来酸双酯，加入三口烧瓶中，用质量分数为40%的氢氧化钠溶液将其pH中和至7，加入3.1-4.3质量份十二烷基磺基琥珀酸酯二钠盐；Weigh 9.3-10.8 parts by mass of fatty acid monoethanolamide maleic acid diester, add it to a three-necked flask, neutralize its pH to 7 with a sodium hydroxide solution with a mass fraction of 40%, and add 3.1-4.3 parts by mass of twelve Alkyl sulfosuccinate disodium salt;

称取2.2-2.4质量份的亚硫酸氢钠，并且将其配成30%的亚硫酸氢钠溶液滴加到三口烧瓶中，在70-80℃的水浴锅中使体系搅拌均匀；将反应物转入微波消解仪中在温度140℃-180℃、功率600W的条件下反应40-90min得到脂肪酸单乙醇酰胺磺基琥珀酸双酯；Weigh 2.2-2.4 parts by mass of sodium bisulfite, and make 30% sodium bisulfite solution dropwise into a three-necked flask, and stir the system evenly in a water bath at 70-80°C; Transfer to a microwave digestion apparatus and react for 40-90min at a temperature of 140°C-180°C and a power of 600W to obtain fatty acid monoethanolamide sulfosuccinic acid diester;

步骤二：制备含羧基-磺酸基不对称Gemini表面活性剂：Step 2: Preparation of asymmetric Gemini surfactants containing carboxyl-sulfonic acid groups:

称取3.4-4.2质量份的氯乙酸，配成30%溶液，并将其溶液用氢氧化钠调节pH至7；Weigh 3.4-4.2 parts by mass of chloroacetic acid to make a 30% solution, and adjust the pH of the solution to 7 with sodium hydroxide;

将氯乙酸溶液滴加至18.36-22.44质量份的肪酸单乙醇酰胺磺基琥珀酸双酯后，调节体系pH至7，搅拌均匀；After adding the chloroacetic acid solution dropwise to 18.36-22.44 parts by mass of fatty acid monoethanolamide sulfosuccinic acid diester, adjust the pH of the system to 7, and stir evenly;

将反应物转入高通量微波消解/萃取/合成工作站控制温度70-90℃，功率600w，反应90-120min，每间隔20min测其pH并调节至7，得到一种含羧基—磺酸基不对称Gemini表面活性剂。Transfer the reactant to a high-throughput microwave digestion/extraction/synthesis workstation, control the temperature at 70-90°C, power 600w, react for 90-120min, measure the pH every 20min and adjust it to 7 to obtain a carboxyl-sulfonic acid group-containing Asymmetric Gemini Surfactants.

步骤一中，脂肪酸单乙醇酰胺马来酸双酯选自十二酸单乙醇酰胺马来酸双酯、油酸单乙醇酰胺马来酸双酯、硬脂酸单乙醇酰胺马来酸双酯、菜籽油单乙醇酰胺马来酸双酯。In step one, fatty acid monoethanolamide maleic acid diester is selected from dodecanoic acid monoethanolamide maleic acid diester, oleic acid monoethanolamide maleic acid diester, stearic acid monoethanolamide maleic acid diester, Rapeseed oil monoethanolamide maleate diester.

实施例1：Example 1:

步骤一：称取9.8质量份的脂肪酸单乙醇酰胺马来酸双酯，用40%的氢氧化钠溶液将其pH中和至7，加入3.3质量份十二烷基磺基琥珀酸酯二钠盐。称取2.2质量份的亚硫酸氢钠，并且将其配成30%的亚硫酸氢钠溶液滴加到三口烧瓶中，在70-80℃的水浴锅中使体系搅拌均匀。将反应物转入微波消解仪中在温度170℃、功率600W的条件下反应90min得到脂肪酸单乙醇酰胺磺基琥珀酸双酯。Step 1: Weigh 9.8 parts by mass of fatty acid monoethanolamide maleic acid diester, neutralize its pH to 7 with 40% sodium hydroxide solution, add 3.3 parts by mass of disodium dodecyl sulfosuccinate Salt. Weigh 2.2 parts by mass of sodium bisulfite, and make it into a 30% sodium bisulfite solution dropwise into a three-necked flask, and stir the system evenly in a water bath at 70-80°C. The reactants were transferred to a microwave digestion apparatus and reacted for 90 minutes under the conditions of a temperature of 170° C. and a power of 600 W to obtain fatty acid monoethanolamide sulfosuccinic acid diester.

步骤二：称取3.7质量份的氯乙酸，配成30%溶液，并将其溶液用氢氧化钠调节pH至7。将上述30%氯乙酸溶液滴加至20.44质量份的肪酸单乙醇酰胺磺基琥珀酸双酯后调节体系pH至7，搅拌均匀。将反应物转入高通量微波消解/萃取/合成工作站控制温度90℃，功率600w，反应120min，每间隔20min测其pH并调节至7，得到一种含羧基—磺酸基不对称Gemini表面活性剂。Step 2: Weigh 3.7 parts by mass of chloroacetic acid to prepare a 30% solution, and adjust the pH of the solution to 7 with sodium hydroxide. Add the above 30% chloroacetic acid solution dropwise to 20.44 parts by mass of fatty acid monoethanolamide sulfosuccinic acid diester, adjust the pH of the system to 7, and stir evenly. The reactant was transferred to a high-throughput microwave digestion/extraction/synthesis workstation with a controlled temperature of 90°C and a power of 600w for 120 minutes. The pH was measured every 20 minutes and adjusted to 7 to obtain a carboxyl-sulfonic acid group-containing asymmetric Gemini surface active agent.

步骤一中，脂肪酸单乙醇酰胺为十二酸单乙醇酰胺马来酸双酯。In step 1, the fatty acid monoethanolamide is lauric acid monoethanolamide maleic acid diester.

实施例2：Example 2:

步骤一：称取10.8质量份的脂肪酸单乙醇酰胺马来酸双酯，用40%的氢氧化钠溶液将其pH中和至7，加入4.3质量份十二烷基磺基琥珀酸酯二钠盐。称取2.4质量份的亚硫酸氢钠，并且将其配成30%的亚硫酸氢钠溶液滴加到三口烧瓶中，在80℃的水浴锅中使体系搅拌均匀。将反应物转入微波消解仪中在温度180℃、功率600W的条件下反应60min得到脂肪酸单乙醇酰胺磺基琥珀酸双酯。Step 1: Weigh 10.8 parts by mass of fatty acid monoethanolamide maleic acid diester, neutralize its pH to 7 with 40% sodium hydroxide solution, add 4.3 parts by mass of disodium dodecyl sulfosuccinate Salt. Weigh 2.4 parts by mass of sodium bisulfite, and make a 30% sodium bisulfite solution dropwise into a three-necked flask, and stir the system evenly in a water bath at 80°C. The reactant was transferred to a microwave digestion apparatus and reacted for 60 minutes under the conditions of temperature 180°C and power 600W to obtain fatty acid monoethanolamide sulfosuccinic acid diester.

步骤二：称取3.8质量份的氯乙酸，配成30%溶液，并将其溶液用氢氧化钠调节pH至7。将上述30%氯乙酸溶液滴加至19.6质量份的肪酸单乙醇酰胺磺基琥珀酸双酯后调节体系pH至7，搅拌均匀。将反应物转入高通量微波消解/萃取/合成工作站控制温度85℃，功率600w，反应100min，每间隔20min测其pH并调节至7，得到一种含羧基-磺酸基不对称Gemini表面活性剂。Step 2: Weigh 3.8 parts by mass of chloroacetic acid to prepare a 30% solution, and adjust the pH of the solution to 7 with sodium hydroxide. Add the above 30% chloroacetic acid solution dropwise to 19.6 parts by mass of fatty acid monoethanolamide sulfosuccinic acid diester, adjust the pH of the system to 7, and stir evenly. The reactant was transferred to a high-throughput microwave digestion/extraction/synthesis workstation with a controlled temperature of 85°C and a power of 600w for 100 minutes. The pH was measured every 20 minutes and adjusted to 7 to obtain a carboxyl-sulfonic acid group-containing asymmetric Gemini surface active agent.

步骤一中，脂肪酸单乙醇酰胺为油酸单乙醇酰胺马来酸双酯。In step 1, the fatty acid monoethanolamide is oleic acid monoethanolamide maleic acid diester.

实施例3：Example 3:

步骤一：称取9.3质量份的脂肪酸单乙醇酰胺马来酸双酯，用40%的氢氧化钠溶液将其pH中和至7，加入3.3质量份十二烷基磺基琥珀酸酯二钠盐。称取2.25质量份的亚硫酸氢钠，并且将其配成30%的亚硫酸氢钠溶液滴加到三口烧瓶中，在75℃的水浴锅中使体系搅拌均匀。将反应物转入微波消解仪中在温度160℃、功率600W的条件下反应90min得到脂肪酸单乙醇酰胺磺基琥珀酸双酯。Step 1: Weigh 9.3 parts by mass of fatty acid monoethanolamide maleic acid diester, neutralize its pH to 7 with 40% sodium hydroxide solution, add 3.3 parts by mass of disodium dodecyl sulfosuccinate Salt. Weigh 2.25 parts by mass of sodium bisulfite, and make it into a 30% sodium bisulfite solution dropwise into a three-necked flask, and stir the system evenly in a water bath at 75°C. The reactant was transferred to a microwave digestion apparatus and reacted for 90 minutes under the conditions of a temperature of 160° C. and a power of 600 W to obtain fatty acid monoethanolamide sulfosuccinic acid diester.

步骤二：称取3.4质量份的氯乙酸，配成30%溶液，并将其溶液用氢氧化钠调节pH至7。将上述30%氯乙酸溶液滴加至18.36质量份的肪酸单乙醇酰胺磺基琥珀酸双酯后调节体系pH至7，搅拌均匀。将反应物转入高通量微波消解/萃取/合成工作站控制温度75℃，功率600w，反应90min，每间隔20min测其pH并调节至7，得到一种含羧基—磺酸基不对称Gemini表面活性剂。Step 2: Weigh 3.4 parts by mass of chloroacetic acid to prepare a 30% solution, and adjust the pH of the solution to 7 with sodium hydroxide. Add the above 30% chloroacetic acid solution dropwise to 18.36 parts by mass of fatty acid monoethanolamide sulfosuccinic acid diester, adjust the pH of the system to 7, and stir evenly. Transfer the reactant to a high-throughput microwave digestion/extraction/synthesis workstation, control the temperature at 75°C, power 600w, react for 90 minutes, measure the pH at intervals of 20 minutes and adjust it to 7, and obtain an asymmetric Gemini surface containing carboxyl-sulfonic acid groups active agent.

步骤一中，脂肪酸单乙醇酰胺为硬脂酸单乙醇酰胺或菜籽油单乙醇酰胺马来酸双酯。In step 1, the fatty acid monoethanolamide is stearic acid monoethanolamide or rapeseed oil monoethanolamide maleic acid diester.

脂肪酸单乙醇酰胺马来酸双酯的结构检测结果如下：The structural detection result of fatty acid monoethanolamide maleic acid diester is as follows:

红外检测结果：3444.24 cm-1处可能为样品吸附水-OH的吸收峰；2925 cm-1、2854cm-1为甲基和亚甲基的反对称和对称伸缩振动吸收峰;1601cm-1为酰胺与羧酸盐吸收峰；1735 cm-1为酯的羰基吸收峰；1400cm-1 羧酸根特征峰1240 cm-1、1174 cm-1为-C-O-C-的不对称伸缩振动的吸收峰；1116 cm-1和1047 cm-1是SO3伸缩振动吸收峰。Infrared detection results: 3444.24 cm -1 may be the absorption peak of the sample adsorbed water-OH; 2925 cm -1 and 2854 cm -1 are the antisymmetric and symmetric stretching vibration absorption peaks of methyl and methylene; 1601cm -1 is the amide and carboxylate absorption peak; 1735 cm -1 is the carbonyl absorption peak of ester; 1400 cm -1 carboxylate characteristic peak 1240 cm -1 , 1174 cm -1 is the absorption peak of asymmetric stretching vibration of -COC-; 1116 cm - 1 and 1047 cm - 1 are SO stretching vibration absorption peaks.

本发明的内容不限于实施例所列举，本领域普通技术人员通过阅读本发明说明书而对本发明技术方案采取的任何等效的变换，均为本发明的权利要求所涵盖。The content of the present invention is not limited to the examples listed, and any equivalent transformation of the technical solution of the present invention adopted by those of ordinary skill in the art by reading the description of the present invention is covered by the claims of the present invention.

Claims (1)

1. the microwave preparation containing carboxyl-sulfonic group Asymmetric Gemini surfactants, it is characterised in that：
Realized by following steps：
Step 1：Prepare fatty monoethanol amide sulfosuccinic acid diester：
The fatty monoethanol amide maleic acid diester of 9.3-10.8 mass parts is weighed, adds in three-necked flask, uses mass fraction Its pH is neutralized to 7 for 40% sodium hydroxide solution, adds 3.1-4.3 mass parts lauryl sulfosuccinate acid esters disodium salts；
The sodium hydrogensulfite of 2.2-2.4 mass parts is weighed, and is made into 30% solution of sodium bisulfite and is added drop-wise to three mouthfuls of burnings In bottle, system is set to stir in 70-80 DEG C of water-bath；By reactant be transferred in microwave dissolver 140 DEG C of temperature- 180 DEG C, reaction 40-90min obtains fatty monoethanol amide sulfosuccinic acid diester under conditions of power 600W；
Step 2：Preparation contains carboxyl-sulfonic group Asymmetric Gemini surfactants：
The monoxone of 3.4-4.2 mass parts is weighed, is made into 30% solution, and its solution is adjusted into pH to 7 with sodium hydroxide；
After chloroacetic acid solution is added dropwise into the fat acid single ethanol amide sulfosuccinic acid diester of 18.36-22.44 mass parts, regulation System pH to 7, stirs；
Reactant is transferred to high flux micro-wave digestion/extraction/70-90 DEG C, power 600w of synthetic work stand control temperature, reacted 90-120min, survey its pH at interval of 20min and adjust to 7, obtain a kind of containing carboxyl-sulfonic group dissymmetric Gemini surface work Property agent；
In step 1, fatty monoethanol amide maleic acid diester is selected from lauric acid/dodecanoic acid single ethanol amide maleic acid diester, oleic acid list Glycollic amide maleic acid diester, stearic acid monoethanolamide maleic acid diester, rapeseed oil single ethanol amide maleic acid diester.
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