Method for recovering ferrocene derivatives and ammonium perchlorate from composite solid propellant

A technology of ferrocene derivatives and solid propellants, applied in the direction of perchloric acid, perchlorate, chemical instruments and methods, etc., can solve the problems of poor safety, complicated process, low recovery rate, etc., and achieve high recovery rate , good quality and cheap price

Inactive Publication Date: 2012-03-14
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the research of recovery methods, it is found that the existing pressurization methods using liquid ammonia, liquid nitrogen and other substances have the problems of complex process, poor safety and low recovery rate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Soaking step: soak the composite solid propellant to be treated with dichloromethane, the soaking temperature is 10°C, and the soaking time is 48h;

[0021] Distillation step: take out the composite solid propellant in the dichloromethane, distill the dichloromethane to obtain crude ferrocene derivatives; the ferrocene derivatives are mainly tert-butyl ferrocene and cattosine;

[0022] Purification step: Purify the crude ferrocene derivative by recrystallization method, the solvent used in the recrystallization method is pentane, and the recovery rate reaches 99.3%;

[0023] Extraction step: extract the soaked composite solid propellant in a saturated solution of ammonium perchlorate, the extraction temperature is 40°C, and the extraction time is 24 hours;

[0024] Recrystallization step: take out the composite solid propellant in the extractant, cool the extractant to 0°C to form a supersaturated solution of ammonium perchlorate, recrystallize ammonium perchlorate crys...

Embodiment 2

[0026] Soaking step: soak the composite solid propellant to be treated with 1,2-dichloroethane, the soaking temperature is 80°C, and the soaking time is 1h;

[0027] Distillation step: take out the composite solid propellant in 1,2-dichloroethane, distill 1,2-dichloroethane to obtain crude ferrocene derivatives; ferrocene derivatives are mainly tert-butyl di Ferrocene, Catoxin;

[0028] Purification step: Purify the crude ferrocene derivative by recrystallization method, the solvent used in the recrystallization method is cyclohexane, and the recovery rate reaches 99.3%;

[0029] Extraction step: extract the soaked composite solid propellant in a saturated solution of ammonium perchlorate, the extraction temperature is 90°C, and the extraction time is 3 hours;

[0030] Recrystallization step: take out the composite solid propellant in the extractant, cool the extractant to 0°C to form a supersaturated solution of ammonium perchlorate, recrystallize ammonium perchlorate crysta...

Embodiment 3

[0033] Soaking step: Soak the composite solid propellant to be treated with N,N-dimethylacetamide, the soaking temperature is 60°C, and the soaking time is 8h;

[0034] Distillation step: take out the composite solid propellant in N,N-dimethylacetamide, distill N,N-dimethylacetamide to obtain crude ferrocene derivatives; ferrocene derivatives are mainly tert-butyl Base ferrocene, catocine;

[0035] Purification steps: Purify the crude ferrocene derivatives by sublimation method, and the recovery rate reaches 99.3%;

[0036] Extraction step: extract the soaked composite solid propellant in a saturated solution of ammonium perchlorate, the extraction temperature is 80°C, and the extraction time is 12 hours;

[0037] Recrystallization step: take out the composite solid propellant in the extractant, cool the extractant to 40°C to form a supersaturated solution of ammonium perchlorate, recrystallize ammonium perchlorate crystals, and the recovery rate reaches 99.5%.

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Abstract

The invention provides a method for recovering ferrocene derivatives and ammonium perchlorate from a composite solid propellant, which belongs to the field of fabrication of composite solid propellants. The method comprises an immersion step of immersing the composite solid propellant in dichloromethane, 1,2-dichloroethanes or N,N-dimethylacetamide, a distillation step of distilling an organic solvent so as to obtain a crude product of ferrocene derivatives, a purification step of purifying the crude product of ferrocene derivatives through recrystallization or sublimation, an extraction step of using a saturated solution of ammonium perchlorate as an extractant and a recrystallization step for obtaining ammonium perchlorate. According to the invention, the method of organic solvents is utilized in the invention for separation and recovery the active components of ammonium perchlorate and ferrocene derivatives, and a high recovery rate is achieved; implementation process of the invention is simple, and the method is easy to form a flow and has a good industrial prospect.

Description

technical field [0001] The invention belongs to the field of composite solid propellant manufacture, in particular to a method for recovering ammonium perchlorate and ferrocene derivative components from composite solid propellant. Background technique [0002] Composite solid propellant is a polyurethane material containing aluminum powder, ammonium perchlorate and ferrocene derivatives in the formula. Waste products and waste materials will be generated during the production process. After the qualified composite solid propellant exceeds the service life Automatic scrapping, therefore, there is a large amount of scrapped composite solid propellants at home and abroad. According to reports, in terms of research and disposal of waste composite solid propellants, there are currently three main methods: such as incineration, blasting, heat recovery, etc.; recycling centered on components such as ammonium perchlorate and aluminum; and designing new types with recyclable functio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/02C01B11/18
Inventor 武德珍刘伟吴战鹏齐胜利汪晓东崔瑞禧胡建军丁敦辉黄刘华
Owner BEIJING UNIV OF CHEM TECH
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