Vinylferrocene oligomer catalyst for catalyzing decomposition of ammonium perchlorate

A technology of vinyl ferrocene and ammonium perchlorate, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical/physical processes, etc., can solve volatile, ferrocene Low catalyst iron content, reduced impact sensitivity of ferrocene catalyst/ammonium perchlorate binary mixture, etc., to achieve adjustable molecular weight, significant catalytic decomposition effect, and good stability

Active Publication Date: 2016-08-03
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention overcomes the shortcoming that the small molecule ferrocene catalyst is volatile, greatly reduces the impact sensitivity of the ferrocene catalyst / ammonium perchlorate binary mixture, and solves the problem of the low iron content of the polymeric side chain grafted ferrocene catalyst The problem

Method used

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  • Vinylferrocene oligomer catalyst for catalyzing decomposition of ammonium perchlorate
  • Vinylferrocene oligomer catalyst for catalyzing decomposition of ammonium perchlorate
  • Vinylferrocene oligomer catalyst for catalyzing decomposition of ammonium perchlorate

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Experimental program
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Effect test

Embodiment 1

[0020] Under anhydrous and oxygen-free conditions, vinyl ferrocene monomer (5.30 g, 25 mmol), anhydrous THF (20 mL), TMEDA (0.45 mL, 3 mmol) were added to a 100 mL Schlenk bottle. The reaction solution was frozen to -20 to -10°C, and the initiator n-butyllithium solution (0.33mL, 2.5M, 0.83mmol) was added, and the reaction solution turned blood red. After reacting for 8h, anhydrous methanol was added to the reaction system ( 1 mL), the reaction was terminated. Add anhydrous methanol (60mL) to precipitate a precipitate, filter with suction, wash the filter residue with methanol, dissolve the filter residue with dichloromethane, filter to obtain a red polymer solution, evaporate the solvent under reduced pressure, and then use an oil pump to remove the residual solvent. Obtained 4.92 g of yellow amorphous powder with a yield of 93%. Iron content is 26.2%; GPC: Mn=4851g / mol; FT-IR (KBr, mainpeaks): ν (cm -1 ) 3089, 2926, 2853, 1629, 1458, 1411, 1397, 1338, 1106, 1068, 1041, 102...

Embodiment 2

[0022] Only change the amount of n-butyllithium solution in Example 1 to (5mL, 2.5M, 12.5mmol), and other operations are consistent with Example 1. 5.25 g of yellow amorphous powder was obtained with a yield of 100%. Iron content 24.4%; GPC: Mn=442 g / mol. FT-IR (KBr, mainpeaks): ν (cm -1 ) 3089, 2925, 2852, 1632, 1458, 1411, 1338, 1106, 1054, 1037, 1023, 1000, 915, 815, 483; 1 HNMR (300MHz, CDCl 3 )δ4.65~3.90(m, Cp), 3.25~0.75(m, CH-CH 2 ); 13 CNMR (101MHz, CDCl 3 )δ67.66 (Cp), 43.27 (CH-CH 2 ), 31.86 (CH-CH 2 ), 22.77 (CH 3 -CH 2 ), 14.34 (CH 3 -CH 2 ).

Embodiment 3

[0024] Only the amount of n-butyllithium solution in Example 1 was changed to (2.5mL, 2.5M, 6.25mmol), and other operations were consistent with Example 1. 5.24 g of yellow amorphous powder was obtained with a yield of 100%. Iron content 25.7%; GPC: Mn=724 g / mol. FT-IR (KBr, mainpeaks): ν (cm -1 )3090, 2924, 2853, 1630, 1458, 1410, 1338, 1106, 1041, 1023, 999, 814, 482; 1 HNMR (300MHz, CDCl 3 )δ4.80~3.85(m, Cp), 3.25~0.80(m, CH-CH 2 ); 13 CNMR (101MHz, CDCl 3 )δ67.66 (Cp), 43.27 (CH-CH 2 ), 31.86 (CH-CH 2 ), 22.77 (CH 3-CH 2 ), 14.34 (CH 3 -CH 2 ).

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Abstract

The invention discloses a vinylferrocene oligomer catalyst for catalyzing decomposition of ammonium perchlorate. The vinylferrocene oligomer catalyst which has high iron content (24.3-26.3%) and a molecular weight in a range of 400-5000 is synthesized by taking vinylferrocene as a polymerization monomer through anionic polymerization, and thevinylferrocene oligomer catalyst is applied to the catalytic decomposition of the ammonium perchlorate. The catalyst is nonvolatile, has remarkable catalytic effect for the thermal decomposition of the ammonium perchlorate, and has extremely low impact sensitivity (10-14%) with an ammonium perchlorate binary mixture system, wherein the impact sensitivity is far low than the high sensitivity (98%) of commonly used catocene corresponding systems; the catalyst can be used as a new catalyst for catalyzing the decomposition of the ammonium perchlorate, and is applied to various solid propellants and gas generating agents which take the ammonium perchlorate as an oxidizing agent.

Description

technical field [0001] The invention discloses a vinyl ferrocene oligomer catalyst, in particular to a vinyl ferrocene oligomer catalyst for catalyzing the decomposition of ammonium perchlorate. Background technique [0002] Ferrocene derivatives are an important class of organometallic compounds. Ferrocene and its derivatives can catalyze the thermal decomposition of ammonium perchlorate, and realize the high-temperature decomposition of ammonium perchlorate. The exothermic temperature and deflagration temperature decrease, so ferrocene and its derivatives are a good positive burning rate catalyst . At present, ferrocene derivatives have been widely used in various solid propellants and gas generators with ammonium perchlorate as the oxidant. The higher the iron content in the ferrocene catalyst described by Kubota (Kubota, N.Propellants and Explosives: Thermochemical Aspects of Combustion, 2nd, Completely Revised and Extended Edition; John Wiley & Sons Ltd., 2007), the h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07F17/02C06D5/04
CPCB01J31/2295C06D5/04C07F17/02
Inventor 杨军钱暮霜俞艳李晓强凌亦飞
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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