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Method for extracting DM-NIP (dimethyl 5-nitroisophthalate) from Aspergillus niger by separation

A technology of dimethyl nitroisophthalate and Aspergillus niger, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as no biological source reports, and achieve easy cultivation and preservation, The effect of reducing energy consumption and easily obtaining substrates

Inactive Publication Date: 2018-10-16
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

About the preparation of 5-Nitro-isophthalate dimethyl ester, there are bibliographical reports very early, and industrial preparation is mainly by 5-Nitro-isophthalate (5-Nitro-iso-phthalate, NIP) and methanol in H 2 SO 4 Obtained by esterification in the presence of

Method used

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  • Method for extracting DM-NIP (dimethyl 5-nitroisophthalate) from Aspergillus niger by separation
  • Method for extracting DM-NIP (dimethyl 5-nitroisophthalate) from Aspergillus niger by separation

Examples

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Effect test

Embodiment 1

[0036] Embodiment 1: a kind of method utilizing Aspergillus niger to isolate and extract 5-nitroisophthalate dimethyl, the steps are as follows:

[0037] 1) Preparation of extract: Extract Aspergillus niger spore powder with acetone at a weight ratio of 1:4 at a temperature of 75°C and a pressure of 0.5MPa to obtain an extract of Aspergillus niger for 3 hours each time. The extract was evaporated with a rotary evaporator at a temperature of 50°C and a pressure of 0.05 MPa until the organic solvent was evaporated to dryness to obtain an extract;

[0038] 2) Silica gel column chromatography: use petroleum ether to wet-pack the column to obtain a silica gel chromatography column, dissolve the extract in step (1) with acetone solvent and mix the sample with silica gel with a size of 250 mesh, evaporate the solvent and apply it in a dry method sample; according to petroleum ether: acetone = 1:0, 40:1, 20:1, 10:1, 5:1, 2:1, 1:1 and 0:1, the elution is carried out in sequence, and th...

Embodiment 2

[0043] Embodiment 2: a kind of method utilizing Aspergillus niger to isolate and extract 5-nitroisophthalate dimethyl, the steps are as follows:

[0044] 1) Preparation of extract: extract Aspergillus niger spore powder with acetone at a weight ratio of 1:4 at a temperature of 50°C and a pressure of 0 MPa to obtain an extract of Aspergillus niger for 3 hours each time, and extract the extract The solution was rotary evaporated with a rotary evaporator at a temperature of 40°C and a pressure of 0.04 MPa until the organic solvent was evaporated to dryness to obtain an extract;

[0045] 2) Silica gel column chromatography: use petroleum ether to wet-pack the column to obtain a silica gel chromatography column, dissolve the extract in step (1) with acetone solvent and mix the sample with silica gel with a size of 200 mesh, evaporate the solvent and apply it in a dry method sample; according to petroleum ether: acetone = 1:0, 40:1, 20:1, 10:1, 5:1, 2:1, 1:1 and 0:1, the elution is ...

Embodiment 3

[0050] Embodiment 3: a kind of method utilizing Aspergillus niger to isolate and extract 5-nitroisophthalate dimethyl, the steps are as follows:

[0051] 1) Preparation of extract: Extract Aspergillus niger spore powder with acetone at a weight ratio of 1:4 at a temperature of 100°C and a pressure of 1.0MPa to obtain an extract of Aspergillus niger for 3 hours each time. The extract was evaporated with a rotary evaporator at a temperature of 60°C and a pressure of 0.06 MPa until the organic solvent was evaporated to dryness to obtain an extract;

[0052] 2) Silica gel column chromatography: use petroleum ether to wet-pack the column to obtain a silica gel chromatography column, dissolve the extract in step (1) with acetone solvent and mix the sample with silica gel with a size of 300 mesh, evaporate the solvent and apply it in a dry method sample; according to petroleum ether: acetone = 1:0, 40:1, 20:1, 10:1, 5:1, 2:1, 1:1 and 0:1, the elution is carried out in sequence, and t...

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Abstract

The invention discloses a method for extracting DM-NIP (dimethyl 5-nitroisophthalate) from Aspergillus niger by separation. The method comprises the following steps: extraction is performed on spore powder of Aspergillus niger by acetone, an Aspergillus niger extract solution is prepared and concentrated, Aspergillus niger extract is prepared and subjected to chromatography, and DM-NIP is prepared, wherein Aspergillus niger is named xj (Aspergillus niger xj) with the preservation number of CCTCC NO:M 206021. Prepared DM-NIP is biologically sourced and has the characteristics of cheap and easily available substrate, simple and feasible extraction process, environment-friendly production process, few solvent residues, low pollution and easily obtained culture medium.

Description

technical field [0001] The invention relates to a method for extracting dimethyl 5-nitroisophthalate, in particular to a method for separating and extracting dimethyl 5-nitroisophthalate by using Aspergillus niger. Background technique [0002] Aspergillus niger is a common species of fungi, which can survive in a wide temperature and pH range and low humidity, and is widely distributed in food, plant products and soils all over the world. As a generally recognized as safe (GRAS) strain certified by the U.S. Food and Drug Administration (U.S.FDA), Aspergillus niger is widely used in the industrial production of organic acids and enzymes, and has huge potential market value. Aspergillus niger produces citric acid, gluconic acid, gallic acid, oxalic acid, etc., and the main enzymes are amylase, catalase, cellulase, pectinase, and acid protease. Not only that, many metabolites of Aspergillus niger have various important application values. [0003] Dimethyl 5-nitroisophthalat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/57C07C201/16
CPCC07C201/16C07C205/57
Inventor 李祝张素冉江肖洋唐婧红张钦语
Owner GUIZHOU UNIV
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