Multichannel vacuum sublimation apparatus and using method thereof

A sublimation device and multi-channel technology, applied in sublimation, separation methods, chemical instruments and methods, etc., can solve the problems of low purification efficiency, complex structure, large amount of purified samples, etc., achieve convenient collection, avoid pollution, and improve purification efficiency Effect

Pending Publication Date: 2019-10-22
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem solved by this application is that the structure of the existing vacuum sublimation device is complex,

Method used

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  • Multichannel vacuum sublimation apparatus and using method thereof
  • Multichannel vacuum sublimation apparatus and using method thereof
  • Multichannel vacuum sublimation apparatus and using method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0041] See figure 1 , is a schematic structural diagram of the deposition chamber of the multi-channel vacuum sublimation device provided in the embodiment of the present application when the deposition chamber is placed horizontally.

[0042] Specifically, the multi-channel vacuum sublimation device of the embodiment of the present application includes two deposition chambers 2 , two air extraction connection devices 3 and a multi-port normalization valve 7 , and one end of each air extraction connection device 3 is connected to the deposition chamber. port connection of body 2; where, as Figure 7 As shown, the multi-port normalizing valve 7 includes four pipelines 7-1, four on-off valves 7-2, a filter screen 7-3 and an adapter 7-4. After the four pipelines 7-1 are connected in parallel It is connected with the conversion joint 7-4, the four pipelines 7-1 are respectively connected in series with the four on-off valves 7-2, and the four pipelines 7-1 are connected in series...

Embodiment 2

[0066] In this example, the multi-channel vacuum sublimation device of Example 1 is used to test the multi-channel vacuum sublimation device based on the sublimation and purification effects of bibithiazole, bipyridine, and fluorenone compounds. The sample compounds involved are all poorly soluble, The thermal stability is good. Among them, the samples with serial numbers 1 to 3 in Table 1 are bidithiazole compounds, the sample with serial number 4 is a bipyridine compound, and samples 5 to 6 are fluorenone compounds. The specific experimental results are as follows 1 shown.

[0067] Due to the poor solubility of the above compounds, the crude products of the reactants were directly subjected to vacuum sublimation purification; after the first sublimation purification, the purity detection and yield calculation were not carried out, but the secondary sublimation purification was directly carried out, and the NMR or elemental analysis was detected. , the purity of the second su...

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Abstract

The invention relates to the technical field of solid organic compound purification apparatuses, and concretely relates to a multichannel vacuum sublimation apparatus and a using method thereof. The apparatus includes at least two deposition cavities, at least two air exhaust connecting devices and a multiport normalization valve, and one ends of the air exhaust connecting devices are connected with the ports of the deposition cavities; and the multiport normalization valve includes at least two pipelines, an on-off valve and a switching joint, the at least two pipelines are connected in parallel, and then is connected with the switching joint, the on-off valve is arranged between the parallel-connected pipelines and the switching joint, one ends of the pipelines are connected to the air exhaust connecting devices, and the switching joint is used for connecting with a vacuum system. The multichannel vacuum sublimation apparatus has the advantages of flexibility in assembling, low price, small size, easiness in operation, high efficiency, realization of simultaneous vacuum sublimation purifying of multiple samples, easiness in control of conditions, and is suitable for being promoted and used in laboratories such as universities and research institutes.

Description

technical field [0001] The application belongs to the technical field of solid organic compound purification devices, and in particular relates to a multi-channel vacuum sublimation device and a method for using the same. Background technique [0002] In the field of organic chemistry, high-purity organic compound samples are of great scientific significance for molecular structure identification, spectral properties and biological activity studies. For organic compounds with poor solubility, especially small organic molecules containing large π-conjugated systems, it is difficult to separate and purify them by conventional methods such as column chromatography, thin-layer chromatography and recrystallization. Collect and grow crystals by solution method. In addition, the products separated by the solution method often contain the interference of impurities such as organic solvents, water, and silica gel during structural identification, and it is difficult to obtain high-s...

Claims

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Application Information

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IPC IPC(8): B01D7/00
CPCB01D7/00
Inventor 曹少魁贾明李亚波黄萌萌金廷根刘应良吴养洁
Owner ZHENGZHOU UNIV
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