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Preparation method for water-soluble sulfonated calixarene

A sulfonated calixarene, water-soluble technology, applied in the field of preparation of functional compounds, can solve the problems of low product purity, unsatisfactory mixed acids and salts, etc., and achieve the effect of simple purification steps

Active Publication Date: 2020-03-31
SHENZHEN INST OF ADVANCED TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the above-mentioned deficiencies of the prior art, and to provide a preparation method of sulfonated calixarene, aiming at solving the unsatisfactory problems of low product purity, entrapped acid and salt etc. obtained by the existing sulfonated calixarene preparation method

Method used

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  • Preparation method for water-soluble sulfonated calixarene
  • Preparation method for water-soluble sulfonated calixarene
  • Preparation method for water-soluble sulfonated calixarene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 100 mL of concentrated sulfuric acid with a concentration of 98% to a three-port reaction vessel equipped with a temperature-controlled base, then accurately weigh 2 g of calixarene (TCA) and add it to the concentrated sulfuric acid, adjust the temperature of the temperature-controlled base to ensure that the reaction temperature is at 80 ° C, and the reaction A polytetrafluoroethylene stirring paddle was used for stirring in the vessel. During the reaction process, the reaction process is monitored by monitoring the solubility of the reaction solution in water, and the reaction is complete if the reaction solution is completely water-soluble. After reacting for about 20 hours, take a drop of the reaction solution and drop it into 10mL aqueous solution every 1 hour, and observe whether it can be completely dissolved in 10mL water. After 24 hours of final reaction, all the reactants can be dissolved in water, and the solution is clear and transparent, indicating that ...

Embodiment 2

[0033] Add 180mL of concentrated sulfuric acid (98% concentration) to a three-port reaction vessel with a temperature-controlled base, then accurately weigh 3g of calixarene (TCA) and add it to the concentrated sulfuric acid to adjust the temperature of the temperature-controlled base to ensure that the reaction temperature is at 85°C. The reactor is stirred with a polytetrafluoroethylene stirring paddle. During the reaction process, the reaction process is monitored by monitoring the solubility of the reaction solution in water, and the reaction is complete if the reaction solution is completely water-soluble. After reacting for about 15 hours, take a drop of the reaction solution and drop it into 10mL aqueous solution every 1 hour, and observe whether it can be completely dissolved in 10mL of water. After 22 hours of final reaction, all the reactants can be dissolved in water, and the solution is clear and transparent, indicating that the reaction completely. Then cooling t...

Embodiment 3

[0037]Add 60mL of concentrated sulfuric acid (98% concentration) to a three-port reaction vessel with a temperature-controlled base, then accurately weigh 1.0g of calixarene (TCA) and add it to the concentrated sulfuric acid, adjust the temperature of the temperature-controlled base to ensure that the reaction temperature is at 75°C , The reactor is stirred with a polytetrafluoroethylene stirring paddle. During the reaction process, the reaction process is monitored by monitoring the solubility of the reaction solution in water, and the reaction is complete if the reaction solution is completely water-soluble. After reacting for about 20 hours, take a drop of the reaction solution and drop it into 10mL aqueous solution every 1 hour, and observe whether it can be completely dissolved in 10mL water. After 28 hours of final reaction, all the reactants can be dissolved in water, and the solution is clear and transparent, indicating that the reaction completely. Then cool the reac...

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Abstract

The invention relates to a preparation method for water-soluble sulfonated calixarene. The preparation method comprises the following concrete steps: (1) adding calixarene into calculated quantitativeconcentrated sulfuric acid for a sulfonation reaction, and monitoring the reaction progress so as to guarantee completion of the reaction; (2) after the reaction is completed, carrying out cooling toa room temperature, pouring reactants into crushed ice, carrying out extraction so as to obtain a flocculent precipitate, and collecting a solid product so as to obtain a crude sulfonated calixareneproduct; and (3) dissolving the crude sulfonated calixarene product, and carrying out separating and purifying so as to obtain a pure water-soluble sulfonated calixarene product. According to the invention, the optimal concentration of sulfuric acid is adjusted by controlling the optimal ratio of the reactants, i.e., the calixarene to the concentrated sulfuric acid and combining different solubility of a reaction product in a sulfuric acid solution; sodium chloride salt does not need to be added for salting out; meanwhile, the crude product is dissolved and purified to obtain high-purity sulfuric-acid-free water-soluble sulfonated calixarene.

Description

technical field [0001] The invention belongs to the field of preparation of functional compounds, and in particular relates to a water-soluble sulfonated calixarene and a preparation method thereof. Background technique [0002] As we all know, bio-related systems are all under the condition of aqueous solution environment, and many biological processes occur in aqueous solution, so molecular recognition research in aqueous solution will become an inevitable trend in the development of fluorescent sensors, and various fluorescent sensors currently reported Most of molecular recognition studies are limited to a pure organic solvent environment or a mixed system of organic solvent and water. This may be attributed to the natural properties of organic compounds—insoluble in water, and related organic compounds are difficult to derivatize into water-soluble compounds, thus limiting their application range and practical value. Research investigations have shown that calixarene i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D341/00
CPCC07D341/00
Inventor 金宗文赵江林阮琴罗擎颖卫小元
Owner SHENZHEN INST OF ADVANCED TECH
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