Supercharge Your Innovation With Domain-Expert AI Agents!

Method for separating and purifying NONA

A technology of nonanitroterphenyl and purification method, applied in the field of compound separation, can solve the problems of long time-consuming, long time-consuming, complicated operation and the like of nitrobenzene, and achieve the effects of short experimental period, time saving and easy operation.

Inactive Publication Date: 2016-05-04
XIAN MODERN CHEM RES INST
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Steam distillation of nitrobenzene takes a long time, and the operation of fractional crystallization is very difficult. Usually, multiple fractional crystallizations are required to obtain pure 2,2′,2″,4,4′,4″,6,6′,6″- Nonanitroterphenyl, the chromatographic separation operation is cumbersome and time-consuming
Therefore, the separation and refining cycle is long and the operation is complicated, which are the two major factors restricting the development and application of 2,2′,2″,4,4′,4″,6,6′,6″-nonanitroterphenyl

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
  • Method for separating and purifying NONA

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] At room temperature, add 400ml of chloroform to the reaction mother liquor of 100ml 2,2',2",4,4',4",6,6',6"-nonanitroterphenyl, a brownish black solid is precipitated, Filter, wash the filter cake with 100ml of toluene for 4 times until the filtrate is colorless, heat filter, dissolve the filter cake in 100ml of acetone, add 10g of activated carbon, 10g of diatomaceous earth for decolorization, filter, and evaporate the filtrate to obtain 2,2' , 2", 4, 4', 4", 6, 6', 6"-nonanitroterphenyl, yield 16%, purity 98.00% (HPLC).

[0015] Structure Identification:

[0016] 1 HNMR (acetone-d6, 500MHz): 9.346 (s, 4H), 9.457 (s, 1H);

[0017] IR(KBr)γ: 3444, 3108, 1608, 1543, 1340, 1175, 1128, 1076, 921, 824, 726, 541cm -1 .

[0018] The above structural identification data confirm that the substance obtained in this step is 2,2′,2″,4,4′,4″,6,6′,6″-nonanitroterphenyl.

Embodiment 2

[0020] At room temperature, add 500ml of chloroform to the reaction mother liquor of 100ml 2,2',2",4,4',4",6,6',6"-nonanitroterphenyl, a brown-black solid is precipitated, Filter, wash the filter cake with 100ml of toluene for 5 times until the filtrate is colorless, heat filter, dissolve the filter cake in 100ml of acetone, add 10g of activated carbon, 10g of diatomaceous earth for decolorization, filter, evaporate the filtrate to dryness to obtain 2,2' , 2", 4, 4', 4", 6, 6', 6"-nonanitroterphenyl, yield 16%, purity 98.00% (HPLC).

Embodiment 3

[0022] At room temperature, add 300ml of chloroform to the reaction mother liquor of 100ml 2,2',2",4,4',4",6,6',6"-nonanitroterphenyl, and a brown-black solid is precipitated. Filter, wash the filter cake with 100ml of toluene for 4 times until the filtrate is colorless, heat filter, dissolve the filter cake in 100ml of acetone, add 10g of activated carbon, 10g of diatomaceous earth for decolorization, filter, and evaporate the filtrate to obtain 2,2' , 2″, 4, 4′, 4″, 6, 6′, 6″-nonanitroterphenyl, yield 12%, purity 97.00% (HPLC).

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 a method for separating and purifying 2,2',2'',4,4',4'',6,6',6''-NONA. The structural formula of 2,2',2'',4,4',4'',6,6',6''-NONA is shown in the description. The method comprises the steps that an organic solvent is added to mother liquor (containing 2,2',4,4',6,6',6''-HNB, 2,2',2'',4,4',4'',6,6',6''6'''-DODECA, picryl chloride and trinitrodichlorobenzene) of 2,2',2'',4,4',4'',6,6',6''-NONA, 2,2',2'',4,4',4'',6,6',6''-NONA, other products and unreacted raw materials are separated out of the mother liquor, then organic solvent boiling and washing and activated carbon and kieselguhr decoloration are carried out, and pure 2,2',2'',4,4',4'',6,6',6''-NONA is obtained.

Description

technical field [0001] The invention relates to a method for separating compounds, in particular to a method for separating and purifying 2,2', 2", 4, 4', 4", 6, 6', 6"-nonanitroterphenyl. Background technique [0002] 2,2′,2″,4,4′,4″,6,6′,6″-nonanitroterphenyl (NONA) is a kind of heat-resistant explosive with excellent performance, the density is 1.76g / cm 3 , decomposition peak temperature 397℃, impact sensitivity (h 50 ) 39cm, detonation velocity 7560m / s, and the heat-resistant explosive has good crystallization and detonation performance, can detonate 100% at high temperature, and can be used in aerospace flexible detonating cord (MDF), flexible cutting cord (FLSC), ultra-high temperature Booster charge or main charge of petroleum perforating bullets, preferred drug for aerospace, detonating cord for safe detonation, shock plate detonator, variable linear propellant, etc. [0003] 2,2', 2 ", 4,4', 4", 6,6', 6"-nonanitroterphenyl disclosed in U.S. Patent No. 3,755,471 ar...

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): C07C201/16C07C205/06
CPCC07C201/16C07C205/06
Inventor 周杰文张蒙蒙张创军王友兵张媛媛胡琳琳李媛黄凤臣席伟汪强
Owner XIAN MODERN CHEM RES INST
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com