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Method for preparing spherical organic micro-molecular monomer or compound through emulsion technology

A small molecule monomer, spheroidization technology, applied in the direction of organic chemistry, granulation of raw materials, organic active ingredients, etc., to achieve the effect of improving fluidity, reducing sensitivity and cost-effectiveness

Active Publication Date: 2017-05-31
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, most of the research on drug compounding still stays in the basic theoretical aspects such as the detection and analysis of its structure and the selection of compound reagents, and its application research needs to be strengthened, such as changing the melting point of the drug, the solubility of the drug, improving the stability and biological properties of the drug. Utilization and biological activity research and pharmaceutical research, etc.

Method used

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  • Method for preparing spherical organic micro-molecular monomer or compound through emulsion technology
  • Method for preparing spherical organic micro-molecular monomer or compound through emulsion technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Step 1. Feed with hexanitrohexaazaisowurtzitane (CL-20) / p-nitrochlorobenzene (PNCB)=1:3 molar ratio, weigh 0.438g of CL-20 and 0.479g of PNCB respectively Add it to a reaction flask containing 5mL of ethyl acetate, then add 16mL of distilled water, then put it in a stirrer at 40°C and stir at 1000rpm, add 2×10 -4 g surfactant gelatin, after the emulsion is uniformly dispersed, carry out ultrasonic emulsification with a power of 1200W for 60min to obtain a uniformly dispersed emulsion; adopt the method of adding non-solvent ethanol extraction to allow crystals to separate out to obtain a solid-liquid mixture; the non-solvent ethanol The dosage is 10 times the mass of the solute;

[0030] Step 2, filtering, washing and drying the solid-liquid mixture to obtain complex spherical crystals; figure 1 c) SEM schematic of the CL-20 / PNCB complex co-crystal is shown; from figure 1 It can be seen from the figure that the particle size distribution of the CL-20 / PNCB composite eut...

Embodiment 2

[0032] Step 1. Feed materials at a molar ratio of CL-20 / 2,4,6-trinitrotoluene (TNT) / PNCB=1:2:3, and weigh 0.438g CL-20, 0.2g TNT and 0.479g PNCB respectively Add it into a reaction flask containing 7mL of ethyl acetate, then add 28mL of water, then put it in a stirrer at 40°C and stir at 800rpm, add 1.5×10 -4 g surfactant gelatin, after the emulsion is uniformly dispersed, carry out ultrasonic emulsification for 60min with a power of 1200W to obtain a uniformly dispersed emulsion; adopt the method of adding non-solvent ethanol extraction to allow crystals to separate out; obtain a solid-liquid mixture; the non-solvent ethanol The dosage is 15 times the mass of the solute;

[0033] Step 2, the solid-liquid mixture is filtered, washed and dried to obtain complex spherical crystals.

Embodiment 3

[0035] Step 1. Feed materials at a molar ratio of CL-20 / PNCB=1:3, weigh 0.438g of CL-20 and 0.479g of PNCB respectively and add them to a reaction bottle containing 7mL of ethyl acetate, then add 28mL of water , and then placed in a stirrer at 40 ° C with 1000rpm stirring, adding 4 × 10 -4 g surfactant gelatin, after the emulsion is uniformly dispersed, perform ultrasonic emulsification with a power of 1200W for 60 minutes to obtain a uniformly dispersed emulsion; use the method to raise the temperature to 90°C to allow crystals to precipitate; obtain a solid-liquid mixture;

[0036] Step 2, the solid-liquid mixture is filtered, washed and dried to obtain complex spherical crystals.

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Abstract

The invention discloses a method for preparing a spherical organic micro-molecular monomer or compound through an emulsion technology. The method comprises the following steps: adding one or more organic micro-molecules to a solvent-nonsolvent, stirring the one or more organic micro-molecules and the solvent-nonsolvent, adding a surfactant, carrying out ultrasonic or mechanical emulsion after the above obtained emulsion is uniformly dispersed, precipitating crystals through adopting a crystal precipitation technology to obtain a solid and liquid mixture, filtering the mixture, washing the obtained solid, and drying the washed solid to obtain monomer or compound spherical crystals. Compounding, super refinement and spheroidization of the organic micro-molecules are combined in the invention, so the sensitivity of an energetic material is greatly reduced, the fluidity and the loading density of the energetic material are improved, and the viscosity of the crystals in the 3D printing or PBX explosive slurry of the energetic material is reduced; the change of the melting point and the solubility of a medicine improves the stability and the bioavailability of the medicine and facilitates pressing into tablets; and the crystals allow the researching and application fields of conductive organic crystals, nonlinear optical crystals, dyes, photograph raw material pigments and agrochemicals to be expanded.

Description

technical field [0001] The invention belongs to material spheroidization technology, in particular to a method for preparing spheroidized small organic molecule monomers and compounds. Background technique [0002] With the changes in the modern war situation, the requirements for explosives are getting higher and higher. While requiring high detonation velocity and high energy, explosives are also required to have better safety, so as to avoid accidents and explosions during transportation and use. . Therefore, the two seemingly contradictory properties of high energy and low sensitivity have become the highest pursuit goals of researchers in the field of energetic materials. At present, the modification methods of desensitization include composite, spheroidization and ultra-fine, etc., due to the interaction between molecules of energetic materials, especially organic small molecule energetic materials and their dangerous characteristics, the realization of the above modi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C06B21/00C06B25/34C06B31/32C06B25/38C06B29/22C06B25/04A61K31/55A61K47/18A61K31/341A61K31/522A61K31/4174A61K31/167A61K31/519A61K31/616A61K31/192A61K31/496C07D307/52B01J2/00C07D223/22
CPCA61K31/167A61K31/192A61K31/341A61K31/4174A61K31/496A61K31/519A61K31/522A61K31/55A61K31/616A61K47/18B01J2/00C06B21/00C06B21/0033C06B21/0066C06B25/04C06B25/34C06B25/38C06B29/22C06B31/32C07B2200/13C07D223/22C07D307/52A61K2300/00
Inventor 郭长平朱燕芳田璐高冰王茜王敦举杨光成
Owner SOUTHWEAT UNIV OF SCI & TECH
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