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Diethyl ether purification method, and method for improving purity of nitrogen-containing organic matter by using diethyl ether

A purification method and a technology of organic matter, applied in ether separation/purification, chemical instruments and methods, organic chemistry, etc., can solve problems such as failure to fundamentally prevent the formation of iodine element, loss of raw materials, and inability to prevent the oxidation of precursor AX, etc. Achieve low cost, reduce the generation of halogen elemental substances, and overcome the effects of oxidation

Inactive Publication Date: 2020-05-15
HANGZHOU MICROQUANTA SEMICON CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method cannot prevent the precursor AX from being oxidized, and cannot fundamentally prevent the generation of iodine simple substance, and there is also the loss of raw materials

Method used

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  • Diethyl ether purification method, and method for improving purity of nitrogen-containing organic matter by using diethyl ether
  • Diethyl ether purification method, and method for improving purity of nitrogen-containing organic matter by using diethyl ether
  • Diethyl ether purification method, and method for improving purity of nitrogen-containing organic matter by using diethyl ether

Examples

Experimental program
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Effect test

Embodiment 1

[0088] 11). Weigh 0.05mol free radical scavenger pentaerythritol tetrakis(3,5-di-tert-butyl-4-hydroxy)phenylpropionate, and dissolve it in 50 mL of chloroform.

[0089] 12). Weigh 0.05mol hydroperoxide decomposer tris(2,4-di-tert-butylphenyl)phosphite and dissolve it in 50mL of acetone.

[0090] 13). Mix the above two solutions, add 100mL of the mixed solution to 2L of ether, oscillate, mix well, place it in a sealed room at room temperature and avoid light for more than a week, and react completely, remove free radicals and peroxyethyl ether in ether, and obtain purified mixed solution of diethyl ether.

[0091] 14). Weigh 10g of methylammonium iodide powder into a beaker, pour 100mL of absolute ethanol, and stir until completely dissolved. Then gradually add the purified diethyl ether mixed solution into the beaker with a separating funnel until the methyl ammonium iodide crystals no longer precipitate, that is, stop the diethyl ether injection, and fully stir for 15 minute...

Embodiment 2

[0097] 21). Weigh 0.1 mol of free radical scavenger 3-(3,5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate, 0.1 mol of hydroperoxide decomposer thiobis Didodecyl propionate, add them to 10L ether, oscillate, mix well, place in airtight and dark place at room temperature for more than one week, complete reaction to remove free radicals and peroxyethyl ether in ether.

[0098] 22). Add 10g of formamidine ammonium iodide powder into the beaker, pour into 100mL of anhydrous methanol, and stir until completely dissolved. Then gradually add the purified diethyl ether mixed solution into the beaker with a separating funnel until the formamidine ammonium iodide crystals no longer separate out, that is, stop the diethyl ether injection, and fully stir for 15 minutes. Suction filtration with a Buchner funnel yielded formamidine ammonium iodide as a solid.

[0099] 23). Repeat step 22) three times to obtain high-quality formamidine ammonium iodide crystals.

[0100] 24). Disperse...

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Abstract

The invention relates to a diethyl ether purification method. The method comprises the following steps: adding a free radical scavenger and a hydroperoxide decomposer into diethyl ether or adding a mixed solution of the free radical scavenger and the hydroperoxide decomposer into diethyl ether to purify the diethyl ether, and then purifying the purified diethyl ether mixed solution after a full reaction by adopting any one of a liquid separation extraction method, a filtering method or a re-evaporation method to obtain purified diethyl ether. The invention also discloses a method for improvingthe purity of the nitrogen-containing organic matter by using diethyl ether, and an application thereof. The diethyl ether used in the method is purified by using the purification method. The purified diethyl ether is used for cleaning the nitrogen-containing organic matter, so active free radicals and peroxydiethyl ether contained in the diethyl ether are removed, and generation of halogen elementary substances in the nitrogen-containing organic halide is effectively reduced, thereby the high-purity nitrogen-containing organic matter is obtained. The methods have the characteristics of simplicity, feasibility, low cost and the like.

Description

technical field [0001] The invention belongs to the technical field of purification of ether and nitrogen-containing organic matter, and relates to a method for purifying ether, a method for improving the purity of nitrogen-containing organic matter by using ether, and an application thereof. Background technique [0002] Organic-inorganic hybrid perovskite (ABX 3 ) solar cells have the advantages of simple preparation process, low cost, and high photoelectric conversion efficiency, and are expected to become a new generation of mainstream photovoltaic technology, replacing traditional silicon-based solar cells. The photosensitive material of perovskite solar cells is mainly composed of nitrogen-containing organic halide precursor AX (A: nitrogen-containing organic compounds such as methylamine, formamidine; X=Cl, Br, I) and lead halide (PbX 2 ) composition, precursors AX and PbX 2 The purity of has a very important impact on the performance of solar cells. In particular,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/06C07C41/46C07C19/07C07C17/392C07C257/12
CPCC07C41/46C07C17/392C07C257/12C07C43/06C07C19/07
Inventor 不公告发明人
Owner HANGZHOU MICROQUANTA SEMICON CO LTD
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