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Method for preparing 1-[di-(2-hydroxyethyl)amino]-3-cardanol oxyisopropanol by one-pot process

A technology of cardanoloxy isopropanol and hydroxyethyl, which is applied in the preparation field of cardanoloxy isopropanol, can solve the problems of complicated operation, low yield, easy emulsification and the like, and achieves simple operation and simplified reaction. effect of steps

Inactive Publication Date: 2012-08-15
HARBIN NORMAL UNIVERSITY
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Problems solved by technology

[0003] The present invention will solve the problems of low yield, complex operation and easy emulsification in the existing method for preparing 1-[two-(2-hydroxyethyl)amino]-3-cardanoloxy isopropanol. A method for preparing 1-[di-(2-hydroxyethyl)amino]-3-cardanoloxy isopropanol in one pot is provided

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  • Method for preparing 1-[di-(2-hydroxyethyl)amino]-3-cardanol oxyisopropanol by one-pot process
  • Method for preparing 1-[di-(2-hydroxyethyl)amino]-3-cardanol oxyisopropanol by one-pot process

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specific Embodiment approach 1

[0007] Specific embodiment one: present embodiment is the method for preparing 1-[two-(2-hydroxyethyl)amino]-3-cardanoloxy isopropanol by one-pot method, specifically as follows:

[0008] 1. First, add cardanol to sodium hydroxide aqueous solution with a mass concentration of 20% to 40%, and heat it from room temperature to 70°C to 100°C, and then stir at a stirring speed of 800 rpm to 1200 rpm and a temperature of 70 ℃~100℃, react for 1h~3h to obtain sodium cardanol; 2. Add [2,3]-(3-hydroxyl-2-nitrogen)indanone and 18-crown in sequence to the sodium cardanol obtained in step 1 -6 and epichlorohydrin, and react at a stirring speed of 800 rpm to 1200 rpm and a temperature of 80°C to 120°C for 3h to 6h to obtain a pre-reaction product; The reaction product was cooled to room temperature, and the pH of the cooled pre-reaction product was adjusted to neutral with dilute hydrochloric acid, then heated from room temperature to 50°C to 90°C, and diethanolamine was added dropwise at a...

specific Embodiment approach 2

[0014] Specific embodiment 2, the difference between this embodiment and specific embodiment 1 is: in step 1, heat from room temperature to 90°C to 98°C, and then stir at a stirring speed of 900 rpm to 1100 rpm and a temperature of 90°C React at ~98°C for 1.5h to 2.5h to obtain sodium cardanol. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0015] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is that in step 2, the stirring speed is 900 rpm to 1100 rpm and the temperature is 90°C to 110°C for 3.5h to After 4.5h, the pre-reaction product was obtained. Others are the same as in the first or second embodiment.

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Abstract

The invention relates to a preparation method of cardanol oxyisopropanol, particularly a method for preparing 1-[di-(2-hydroxyethyl)amino]-3-cardanol oxyisopropanol by a one-pot process. The invention aims to solve the problems of low yield, complex operation and high emulsification tendency in the existing method for preparing 1-[di-(2-hydroxyethyl)amino]-3-cardanol oxyisopropanol. The method comprises the following steps: 1. preparing sodium cardanol; 2. adding [2,3]-(3-hydroxy-2-nitrogen)hydrindone-18-crown-6 and epoxy chloropropane to obtain a pre-reaction product; 3. adding diethanolamine to obtain a final reaction product; and 4. purifying sequentially by a rotary evaporation method, water-ethanol mixed solvent washing and silicagel column chromatography to obtain the fine 1-[di-(2-hydroxyethyl)amino]-3-cardanol oxyisopropanol product. The invention is mainly used for preparing the 1-[di-(2-hydroxyethyl)amino]-3-cardanol oxyisopropanol.

Description

technical field [0001] The invention relates to a preparation method of cardanol oxy-isopropanol. Background technique [0002] Cardanol is the main component of cashew nut oil, which contains 90% in cashew nut oil. It is an excellent sustainable biomass resource. Because its structure contains phenol structure and unsaturated side chains, many compounds with special uses can be derived , to replace petroleum product phenol to prepare polymer materials such as phenolic resin and polyurethane, which are widely used in automobiles, electronics, construction, ships and other fields. They are environmentally friendly biomaterials and are of great significance in scientific research and industrial production. Polyols are indispensable substances in the preparation of polyurethane products. 1-[di-(2-hydroxyethyl)amino]-3-cardanoloxy isopropanol was synthesized by cardanol, which is a polyhydroxy compound containing three hydroxyl groups and can be used to prepare polymer material...

Claims

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Application Information

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IPC IPC(8): C07C217/32C07C213/04
Inventor 金英学于沙沙曲凤玉梁波颖魏树权谭广慧
Owner HARBIN NORMAL UNIVERSITY
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