Solution-mediated polymorphic transformation of CL-20: An approach to prepare purified form ε particles

Pan, Bochen; Wei, Hongyuan; Jiang, Junwei; Zong, Shanghong; Lv, Penghao; Dang, Leping

doi:10.1016/j.molliq.2018.05.121

Cited by 31 publications

(19 citation statements)

References 42 publications

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“…In situ measurement of solid and solution was used to obtain the solubility measurements. 17 The in situ Raman method typically involves producing a solution of known concentration/composition and varying the temperature until the point of equilibrium is reached, where crystals neither dissolve nor grow. 18 The in situ Raman method requires examining for the point of equilibrium under isothermal conditions, where the solution concentration is varied for each experiment.…”

Section: ■ Experimental Sectionmentioning

confidence: 99%

“…In order to measure the solubility of the β-form, an experimental setup previously developed to investigate solution-mediated phase transitions of HNIW poymorphs was used. , The setup consists of a Raman spectrometer (Kaiser Optical Systems, Ann Arbor MI, USA) used in conjunction with a temperature controller (±0.1 °C) in a jacketed vessel. The vessel was used to hold and seal a quiescent solution sample in which a single crystal of the β-form could be observed.…”

Section: Experimental Sectionmentioning

confidence: 99%

“…The vessel was used to hold and seal a quiescent solution sample in which a single crystal of the β-form could be observed. In situ measurement of solid and solution was used to obtain the solubility measurements . The in situ Raman method typically involves producing a solution of known concentration/composition and varying the temperature until the point of equilibrium is reached, where crystals neither dissolve nor grow .…”

Section: Experimental Sectionmentioning

confidence: 99%

“…where R is the gas constant, Δ dis H, Δ dis S are the dissolution enthalpy and entropy, respectively, and T is the absolute temperature. The value of dissolution enthalpy and dissolution entropy calculated from the slope and intercept in eq 7 are listed in Tables 15,16,17,18,19,and 20. These data show that the Δ dis H of β-HNIW in each binary solvent mixture is exothermic.…”

mentioning

confidence: 94%

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Solubility Measurement Study on a Metastable Polymorph of β-2,4,6,8,10,12-Hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane by Raman Spectroscopy

Park

Yang

Kim

et al. 2019

Crystal Growth & Design

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Raman spectroscopy was used to measure the solubility of the metastable form of β-2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (β-HNIW) in organic binary solvent mixtures. The distinct Raman spectra peaks of the solid, solute, solution, and solvent were investigated. Peaks that were not overlapping each other were used to develop a calibration curve. Then, linear relationships between solution concentration and Raman intensity were used to measure the solubility of β-HNIW in binary solvent mixtures during the dissolving process. The solubility of β-HNIW in binary solvent mixtures (ethyl acetate + n-hetpane, ethyl acetate + 1,1,2-trichloroethane, ethyl acetate + cyclohexane, ethyl acetate + toluene, ethyl acetate + diethyl ether, and ethyl acetate + petroleum ether) was investigated. The temperature ranged from 283.15 K to 333.15 K at atmospheric pressure. The solubility of β-HNIW in binary solvent mixtures decreases with increasing temperature. In order to correlate the solubility of β-HNIW, the combined nearly ideal binary solvent/Redlich–Kister (CNIBS/R-K) model and Jouyban–Acree model were employed. The Jouyban–Acree model is in better agreement with experimental solubility for all of the binary solvent mixtures. The average relative error is less than 0.05. Dissolution enthalpy and entropy were determined using the van’t Hoff equation.

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Section: ■ Experimental Sectionmentioning

confidence: 99%

Section: Experimental Sectionmentioning

confidence: 99%

Section: Experimental Sectionmentioning

confidence: 99%

mentioning

confidence: 94%

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Solubility Measurement Study on a Metastable Polymorph of β-2,4,6,8,10,12-Hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane by Raman Spectroscopy

Park

Yang

Kim

et al. 2019

Crystal Growth & Design

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“…The mechanism controlling the transformation rate is determined by either a growth-controlled process (growth in a stable form) or a dissolution-controlled process (dissolution in a metastable form). − When the metastable phase is formed first, the transformation of the metastable phase into the stable phase follows. Kinetic studies of transformation into an amorphous crystalline form are rarely reported, and the kinetic and rate-controlling steps of phase transformation of GMP are not reported at all, especially for various different operating conditions.…”

Section: Introductionmentioning

confidence: 99%

Dissolution and Growth Kinetics and the Rate-Controlling Step in Transformation of Amorphous to Crystalline Phase Using Antisolvent Crystallization

Kim

Ulrich

2022

Ind. Eng. Chem. Res.

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The kinetics of the formation of amorphous disodium guanosine 5′-monophosphate and its transformation to the heptahydrate phase were studied under various operating conditions using in situ Raman and focused beam reflectance measurement (FBRM). Supersaturation, solvent composition, feed concentration, addition rate, and viscosity were shown to affect the rate-determining steps of the transformation. The rate-controlling mechanisms in the overall kinetics have been confirmed. The observation of the slurry viscosity of the suspension of the amorphous phase shows the option to observe the phase transformation. The transformation process was affected by the dissolution, growth, and supersaturation in which the rate-controlling step was divided into two sections, such as the initial and later sections of the transformation. The overall rate constants were determined by combining the constants of the dissolution rate and the growth rates of each section. In situ Raman spectroscopy examination of the concentration of solution and solids can determine the rate-limiting processes during the transformation. The zero-order, first-order, and surface reaction equations as kinetic equations are highlighted and compared for the dissolution of the amorphous solids and the growth of the heptahydrate crystals. The dissolution of the amorphous (metastable form) and the growth of the heptahydrate (stable form) were found to be best fitted to the zero-order kinetic model. In particular, the variation of particle size distribution over time can give the rate-determining steps. These results suggest that the data measured by Raman spectroscopy and FBRM can be successfully coupled into a dissolution and growth model to further grasp and interpret the phase transformation. A dissolution rate-controlling step was dominated by a pattern in which both supersaturation and amorphous dissolution decreased simultaneously, and the growth rate-controlling step was shown in a pattern in which either supersaturation or amorphous dissolution was constant. Furthermore, the growth of heptahydrate crystals at a viscosity of the suspension with the amorphous solids below 70 cp and the dissolution of the amorphous solids above it can be used as the key determinant. Using the method developed and the kinetic constants obtained in this work, it is possible to create an appropriate control strategy to produce the desired form in the final product.

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Application and Properties of CL‐20/HMX Cocrystal in Composite Modified Double Base Propellants

Liu

Zheng

et al. 2019

Propellants Explo Pyrotec

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The composite modified double base (CMDB) propellants containing 2,4,6,8,10,12‐hexanitro‐2,4,6,8,10,12‐hexaazatetracyclo[5.5.0.05,9.03,11] dodecane (CL‐20), 1,3,5,7‐tetranitro‐1,3,5,7‐tetrazocane (HMX) or CL‐20/HMX cocrystal were prepared by the solventless extrusion formation technique. The performances of CMDB propellants were evaluated by means of stability, sensitivity, combustion and mechanical experiments. Raman spectra analysis indicated the stability of CL‐20/HMX cocrystal is partially destroyed in the rolling process under 90 °C, 10 MPa. Methyl violet tests revealed that the colored time of CMDB propellants containing CL‐20/HMX cocrystal, CL‐20 or HMX are 77, 60, and 75 min, respectively. Burning rate tests shown that the burning rates of CMDB propellants containing CL‐20/HMX cocrystal, CL‐20 or HMX in the pressure range of 8 to 18 MPa, increased 1.82, 4.67, and 4.67 mm/s, with the pressure exponents 0.095, 0.306, and 0.346, respectively. Mechanical property tests revealed that the mechanical properties of CMDB propellant containing CL‐20/HMX cocrystal are inconsistent, but the tensile strength has improved compare with CMDB propellant containing CL‐20. These results suggest that CL‐20/HMX cocrystal is a potential material to solve the application problem of the safety performance and stability of the propellants containing CL‐20.

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Solution-mediated polymorphic transformation of CL-20: An approach to prepare purified form ε particles

Cited by 31 publications

References 42 publications

Solubility Measurement Study on a Metastable Polymorph of β-2,4,6,8,10,12-Hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane by Raman Spectroscopy

Solubility Measurement Study on a Metastable Polymorph of β-2,4,6,8,10,12-Hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane by Raman Spectroscopy

Dissolution and Growth Kinetics and the Rate-Controlling Step in Transformation of Amorphous to Crystalline Phase Using Antisolvent Crystallization

Application and Properties of CL‐20/HMX Cocrystal in Composite Modified Double Base Propellants

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