Method for testing hygroscopicity of 3,4-dinitropyrazole

A technology of dinitropyrazole and testing methods, which is applied in chemical method analysis, measuring devices, and the use of substance absorption and weighing, etc., can solve problems such as restricting applications, and achieve the effects of simple operation, accurate data, and avoiding weighing errors

Pending Publication Date: 2022-01-21
ZHONGBEI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The DNP obtained by this method is affected by certain environmental conditions and has obvious hygroscopicity, which will greatly restrict its application.

Method used

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  • Method for testing hygroscopicity of 3,4-dinitropyrazole
  • Method for testing hygroscopicity of 3,4-dinitropyrazole
  • Method for testing hygroscopicity of 3,4-dinitropyrazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A kind of test method of 3,4-dinitropyrazole hygroscopicity, comprises the following steps:

[0023] (1) DNP solid samples obtained by N-nitration, thermal rearrangement, and C-nitration at room temperature were dried in a vacuum oven at 55°C and a vacuum of 0.1MPa for 3 hours to constant weight, and about 1g of the sample was passed through Karl Fischer moisture titrator titration determined water content at 0.018%;

[0024] (2) Divide the sample into several groups of samples, each group weighs 1.0000±0.0005g of the sample, puts it in a weighing box of known weight that has been washed and dried in advance, and records the total mass of each portion; put the weighing box Take off the lid and put it in a constant temperature and humidity box, set a fixed temperature and relative humidity for moisture absorption for a specified time, seal the lid and put it in a desiccator to cool down to room temperature as a whole, weigh and calculate the moisture absorption rate.

...

Embodiment 2

[0028] A kind of test method of 3,4-dinitropyrazole hygroscopicity, comprises the following steps:

[0029] (1) DNP solid samples obtained by N-nitration, thermal rearrangement, and C-nitration at room temperature were dried in a vacuum oven at 50°C and a vacuum of 0.08MPa for 2h to constant weight, and about 1g of the sample was passed through Karl The moisture content was determined to be 0.02% by Fischer moisture titrator titration;

[0030] (2) Weigh a sample of 1.0000±0.0005g, place it in a weighing box of known weight that has been washed and dried in advance, and record the total mass; then remove the cover of the weighing box and put it in a constant temperature and humidity box , set the temperature at 30°C, the relative humidity at 50%, and the moisture absorption time at 24 hours, and calculate the moisture absorption rate of the sample to be 1.0%.

Embodiment 3

[0032] A kind of test method of 3,4-dinitropyrazole hygroscopicity, comprises the following steps:

[0033] (1) DNP solid samples obtained through N-nitration, thermal rearrangement, and C-nitration at room temperature were dried in a vacuum oven at 53°C and a vacuum of 0.09MPa for 2.5h to constant weight, and about 1g of the sample was collected by Karl Fischer moisture titrator titration determines the water content at 0.015%;

[0034] (2) Weigh a sample of 1.0000±0.0005g, place it in a weighing box of known weight that has been washed and dried in advance, and record the total mass; then remove the cover of the weighing box and put it in a constant temperature and humidity box , set the temperature at 40°C, the relative humidity at 75%, and the moisture absorption time at 48 hours, and calculate the moisture absorption rate of the sample to be 3.4%.

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Abstract

The invention provides a method for testing hygroscopicity of 3,4-dinitropyrazole, which comprises the following steps: drying a 3,4-dinitropyrazole sample to constant weight under a vacuum condition; sampling and measuring the water content of the sample dried in the step 1, and when the mass fraction of water in the sample is greater than 0.02%, continuously drying the sample until the mass fraction of water is less than or equal to 0.02%; sampling the material, carrying out a hygroscopicity experiment under the condition of constant temperature and humidity, and recording the mass and moisture absorption rate of the sample after moisture absorption. The method for testing hygroscopicity of 3,4-dinitropyrazole has the advantages of accurate data and simplicity and convenience in operation. For example, in drying process, the drying time is determined by determining the overall constant weight of a sample in the conventional method, and the specific water content is obtained by titrating a small amount of sample by using a water titrator, so that weighing errors caused by the temperature of the sample are avoided, and meanwhile, specific data of the drying degree of the sample can be obtained.

Description

technical field [0001] The invention relates to the field of energetic materials, in particular to a method for testing the hygroscopicity of 3,4-dinitropyrazole. Background technique [0002] 3,4-Dinitropyrazole (DNP) is an energetic compound of nitroazoles with a melting point of 85°C and a density of 1.87 g cm -3 , the molecular formula is C 3 h 2 N 4 o 4 , with a molecular mass of 158, is a white crystalline solid, easily soluble in compounds such as acetonitrile and methanol at room temperature, has the advantages of low melting point, high density, high nitrogen content, high detonation velocity, and good oxygen balance, and can be used as a carrier for melt-cast explosives. [0003] The DNP synthesis method disclosed in "Synthesis and Characterization of Three New Types of Low-melting Point Explosives" ("Journal of Military Engineering", No. 34, 2013, P36-40) uses pyrazole as a raw material in acetic anhydride-acetic acid-fuming nitric acid In the system, N-nitro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/02G01N31/16
CPCG01N5/025G01N31/168
Inventor 赵林秀张桐伟方克雄李翀申帆帆曹端林李永祥肖芸李敏王建龙龚磊潘红霞陈军刘艳丽刘永政郑入水王艳红任福德陈芳马忠平
Owner ZHONGBEI UNIV
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