Unlock instant, AI-driven research and patent intelligence for your innovation.

Extraction separation method of high-purity cucurbituril Q[7]

A seven-membered melon ring and separation method technology, applied in the chemical field, can solve problems such as high labor intensity, reduced thermal stability, and large consumption of organic reagents, and achieve the effects of rapid separation method, cost saving, and good yield

Active Publication Date: 2015-08-26
北京传奇优声文化传媒有限公司
View PDF12 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing bibliography methods have acid-moisture step method, glycerol separation method, cation exchange resin method, but the purity of the seven-membered melon ring obtained by separation with these methods is not very high, only about 90%-93%, see the appendix figure 2 , with Figure 4 As shown, the seven-membered melon rings are always mixed with a small amount of six-membered melon rings and five-membered melon rings that cannot be removed
Impure seven-membered melons will lead to a decrease in the solubility of the seven-membered melons (1×10 -3 mol / L, the thermal stability is also reduced, which greatly restricts the in-depth study of the seven-membered melon ring
If these methods are used to repeatedly separate and purify the seven-membered melon ring, the purity of the melon ring can reach more than 95%, but the labor intensity is very large, the consumption of organic reagents is large and the yield is only about 10%.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Extraction separation method of high-purity cucurbituril Q[7]
  • Extraction separation method of high-purity cucurbituril Q[7]
  • Extraction separation method of high-purity cucurbituril Q[7]

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 Extraction and separation of high-purity seven-membered melon rings.

[0027] (1) Sample preparation: Dissolve 500 mg of seven-membered melon rings containing five- and six-membered melon rings and a small amount of other impurities obtained by conventional separation methods in 30 mL of water, stir at 40°C for 10 min, filter, and use the filtrate for later use;

[0028] (2) Preparation of chromatographic column: Add 100g of MCIGEL CHP20P reversed-phase chromatographic packing (American Chromatography Company) into 200 mL of methanol for 15 minutes, pour out the methanol, then add 200 mL of double distilled water for 15 minutes, pour out the aqueous solution, and then add appropriate amount of distilled water. Sub-distilled water makes the stationary phase slurry, pour the stationary phase into a glass column with a diameter of 3 cm and a height of 50 cm, rinse with 1000 mL of sub-distilled water and set aside;

[0029] (3) Slowly add 30 mL of the above-mentione...

Embodiment 2

[0033] Example 2 Recycling of impure seven-membered melon rings.

[0034] The fractions detected as impure seven-membered melon ring in Example 1 were combined several times to a total of 2000 mL, concentrated by rotary evaporation at 65°C to a volume of 50 mL, cooled to room temperature and then added with 400 mL of methanol to obtain a white precipitate, suction filtered, and precipitated After washing with 20 mL of methanol and 20 mL of acetone, place it in a vacuum desiccator and dry at 70°C for 12 hours to obtain an impure seven-membered melon ring product, which mainly contains five- and six-membered melon rings. Weigh 4g of the sample, add 500mL double-distilled water and stir for 30 minutes, then filter to remove the precipitate, the filtrate is concentrated by rotary evaporation at 65°C to a volume of 20mL, after cooling to room temperature, add 200mL methanol to obtain a white precipitate, filter with suction, and use 20mL methanol for the precipitate, After washing ...

Embodiment 3

[0035] Example 3 Regeneration of chromatographic column

[0036] Regeneration of the chromatographic column: Rinse the chromatographic column with 600mL of acetic acid aqueous solution with a volume ratio of 20% at a flow rate of 1mL / min, and then rinse with 2000mL of twice distilled water to regenerate the chromatographic column for the next separation. When used more than 6 times, it must be thoroughly cleaned and regenerated to ensure the recovery of the pore size of the chromatographic stationary phase filler. The specific method is as follows: the fixed flushing flow rate is 1mL / min, and the acetic acid aqueous solution with a volume ratio of 20% is 600mL, and the double distilled water is 2000mL. , 400mL of 20% methanol aqueous solution by volume, 400mL of 50% methanol aqueous solution by volume, 400mL of 80% methanol aqueous solution by volume, 400mL of pure methanol, 400mL of 50% methanol aqueous solution by volume, and 1000mL double distilled water. The column can the...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to an extraction separation method of high-purity cucurbituril Q[7], and elates to a cucurbituril Q[7] extraction separation method in the field of supramolecular chemistry. According to the invention, cucurbituril Q[7] containing cucurbituril Q[5], cucurbituril Q[6] and a small amount of other impurities obtained with a conventional separation method is separated and purified with a reverse phase chromatographic method, such that the purity of cucurbituril Q[7] reaches 99% or higher. The extraction separation method is simple and fast, and does not adopt an organic solvent as a mobile phase. The method is environment-friendly, and causes no pollution. The obtained cucurbituril Q[7] product has high purity and good yield. A used chromatographic column can be repeatedly used after treatments, such that cost is low.

Description

technical field [0001] The invention belongs to a chromatographic separation method in the field of chemistry. Specifically, the seven-membered melon rings containing five- and six-membered melon rings and a small amount of other impurities obtained by conventional separation methods are separated and purified by reverse phase chromatography, so that the purity of the seven-membered melon rings can reach 99% or more. Background technique [0002] Cucurbitan chemistry is an emerging discipline in the field of supramolecular chemistry, which has only been developed for decades, but its excellent physical and chemical properties make it useful in supramolecular catalysis, supramolecular assembly, molecular recognition, ion channels, supramolecular Biology, nanoscience, supramolecular pharmacology and other fields show broad application prospects. At the same time, its application has also penetrated into hot fields in the 21st century, such as environmental science, life scien...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 董南
Owner 北京传奇优声文化传媒有限公司