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Online detection method of crystal-transformation reaction endpoint in production process of cyclotetramethylene tetranitramine

An Oktokin and reaction end point technology, applied in the field of explosives, can solve problems such as quality accidents, product purity, unstable quality, inaccuracy, timely guidance and optimization of production processes, etc., to ensure quality and overcome time lag Effect

Inactive Publication Date: 2013-11-27
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The crystal transformation reaction is to convert the unstable α crystal form HMX into a stable β crystal form HMX. The existing process determines the end point of the crystal transformation reaction based on process or experience, and lacks on-site and online detection methods.
Failure to accurately and timely guide and optimize the production process leads to unstable product purity and quality, and even quality accidents

Method used

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  • Online detection method of crystal-transformation reaction endpoint in production process of cyclotetramethylene tetranitramine
  • Online detection method of crystal-transformation reaction endpoint in production process of cyclotetramethylene tetranitramine
  • Online detection method of crystal-transformation reaction endpoint in production process of cyclotetramethylene tetranitramine

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Embodiment 1

[0095] This embodiment provides an on-line detection method for the end point of the crystal transformation reaction in the production process of Oktokin, the method includes the following steps:

[0096] Step 1, collect the near-infrared spectrum of the sample:

[0097] Take a sample of Octogen known to contain α crystal form in the Octogen transformation reaction system, take a sample of Octogen known to contain α crystal form in the crystal transformation reaction system Near-infrared spectrum scanning is carried out on samples of Octogen-type Octogen, and near-infrared spectrum scanning is performed on samples of Octogen that are known not to contain α crystals. -1 , scan times 32 times, resolution 8cm -1 , to obtain the near-infrared spectrum of the sample known to contain the α crystal form of Octogen as shown in figure 1 As shown, the near-infrared spectrum of a sample of Octogen that is known to be free of α crystal form is obtained as figure 2 , recorded as the or...

Embodiment 2

[0133] This embodiment provides an on-line detection method for the end point of the crystal transformation reaction in the production process of Oktokin, the method includes the following steps:

[0134] Step 1, collect the near-infrared spectrum of the sample:

[0135] The method of step 1 and step 2 in the present embodiment is the same as the method of step 1 and step 2 in embodiment 1, obtains the near-infrared spectrum of the sample known to contain linear ammonium nitrate such as figure 1 As shown, the near-infrared spectrum of a sample known to contain no linear ammonium nitrate was obtained as figure 2 As shown, it is recorded as the original spectrum, and the best modeling interval is obtained.

[0136] Step 3, preprocessing of the original spectrum:

[0137] The standard normal variable transformation is performed on the collected original spectrum to obtain the near-infrared spectrum map after the standard normal variable transformation. The standard normal vari...

Embodiment 3

[0148] This embodiment provides an on-line detection method for the end point of the crystal transformation reaction in the production process of Oktokin, the method includes the following steps:

[0149] Step 1, collect the near-infrared spectrum of the sample:

[0150] The method of step 1 and step 2 in the present embodiment is the same as the method of step 1 and step 2 in embodiment 1, obtains the near-infrared spectrum of the sample known to contain linear ammonium nitrate such as figure 1 As shown, the near-infrared spectrum of a sample known to contain no linear ammonium nitrate was obtained as figure 2 As shown, it is recorded as the original spectrum, and the best modeling interval is obtained.

[0151] Step 3, preprocessing of the original spectrum:

[0152] Carry out any combination of smoothing, differential processing, standard normal variable transformation and multivariate scattering correction to the original spectrum, and the specific smoothing, differenti...

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Abstract

The invention belongs to the field of explosives and provides an online detection method of a crystal-transformation reaction endpoint in a production process of cyclotetramethylene tetranitramine. The online detection method comprises the following steps of: acquisition of a near infrared spectrum of a sample, selection of an optimal modeling interval, pretreatment of an original spectrum, and establishment of a model by adopting main-component analysis and online detection of the crystal-transformation reaction endpoint. The online detection method provided by the invention has the advantages that a near infrared technology is used for determining the crystal-transformation reaction endpoint in the production process of the cyclotetramethylene tetranitramine, online determination of the endpoint of an energetic material in the synthesis process is realized, field detection and monitoring of the energetic material in the synthesis process are realized, the quality of a product is ensured, the defect of time delay in the existing detection method of the crystal-transformation reaction endpoint in the production process of the cyclotetramethylene tetranitramine is overcome, the online control for the crystal-transformation reaction process is realized, the safety and the stability of the production process are achieved, and the online detection method is very important for the quality control in the synthesis process of the energetic material.

Description

technical field [0001] The invention belongs to the field of explosives and relates to Octogen, in particular to an on-line detection method for the end point of the crystal transformation reaction in the Octogen production process. Background technique [0002] Octojin (abbreviated as HMX) is the explosive with the best comprehensive performance. It is widely used in mixed explosives, solid propellants and aerospace technology. Real-time monitoring of important quality parameters of key reaction units in the HMX production process, timely acquisition of quality information, real-time optimization and adjustment of production processes are of great significance to ensure product quality and production safety, and are continuous and automated technical support. [0003] The urea synthesis HMX process has the characteristics of low cost and high yield, and has broad prospects for popularization and application. The existing online monitoring methods of this process line only m...

Claims

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Application Information

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IPC IPC(8): G01N21/35
Inventor 张皋蒋忠亮苏鹏飞贾林刘志伟
Owner XIAN MODERN CHEM RES INST
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