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Preparation method of open-celled high-energy molecular microspheres

A technology of polymer microspheres and open-pore structure, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of difficulty in controlling pore size and pore distribution, high toxicity of nitromethane, and high cost of nitromethane, and achieve easy control. , the effect of low toxicity and reduced energy consumption

Active Publication Date: 2015-04-29
NANJING UNIV OF SCI & TECH
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Problems solved by technology

The toxicity of nitromethane is relatively high, and the cost of nitromethane is relatively high
[0004] In addition, the preparation methods of porous energetic polymer spheres that have been publicly reported so far all need to be formed into spheres under heating conditions, and the spherical particles can be completely shaped after the solvent is driven out. These processes will cause changes in the pore structure. Both pore size and pore distribution are very difficult

Method used

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  • Preparation method of open-celled high-energy molecular microspheres
  • Preparation method of open-celled high-energy molecular microspheres
  • Preparation method of open-celled high-energy molecular microspheres

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preparation example Construction

[0024] A method for preparing energetic polymer microspheres with an open-pore structure includes the following steps:

[0025] Step 1. Dissolve the energy-containing polymer material containing nitrocellulose in ethyl acetate to obtain a polymer sol containing nitrocellulose; the energy-containing polymer material containing nitrocellulose is nitrification with a nitrogen content greater than or equal to 11.5% One of cotton, single-base medicine, double-base medicine or modified double-base medicine containing high-energy explosive. The amount of ethyl acetate is 4.0-100 times the mass of the energetic polymer material. The high-energy explosives are elemental explosives such as Roxykin or Oktokin.

[0026] Step 2. Under stirring conditions, gradually add an alkane solvent to the polymer sol described in step 1, and obtain a polymer sol containing a mixed solvent or a polymer emulsion with an alkane solvent as the inner phase after thorough mixing; The alkane solvent is one or a ...

Embodiment 1

[0042] A 2-liter three-necked flask was used as the pelletizing reactor, and nitrocellulose with a nitrogen content of 11.9% and a moisture content of 4% was used as the raw material. The nitrocellulose was added to the reactor, and 20 times the raw material was added under stirring. Dry) quality ethyl acetate solvent, that is, the solvent ratio is 20. After dissolving for 30 minutes, a polymer sol containing nitrocellulose is obtained. Then, 5 times the mass of the crude drug is added to the system, and the mixture is stirred and dispersed for 30 minutes at room temperature. Then continuously add an aqueous solution containing OP-10 non-ionic surfactant to the system. The surfactant concentration in the aqueous solution is 0.25%. The volume of the aqueous solution added is 0.25 times the volume of ethyl acetate in step 1. Continue after the aqueous solution is added Stir for 30 minutes to form a homogeneous polymer emulsion. Next, the polymer emulsion is dispersed in an aqueou...

Embodiment 2

[0044] A 2-liter three-necked flask was used as the pelletizing reactor, and nitrocellulose with a nitrogen content of 11.5% was used as the raw material. The nitrocellulose was added to the reactor, and 10 times the weight of the raw material (dry) was added under stirring. Ethyl acetate solvent, that is, the solvent ratio is 10, after 30 minutes of dissolution, a polymer sol containing nitrocellulose is obtained, and then 4 times the mass of the crude drug is added to the system, and the mixture is stirred and dispersed for 30 minutes at room temperature. Then continuously add an aqueous solution containing cationic surfactant cetyltrimethylammonium chloride to the system, the concentration of cetyltrimethylammonium chloride in the aqueous solution is 0.25%, and the volume of the aqueous solution added is the acetic acid in step 1. 0.4 times the volume of the ethyl ester. After adding the aqueous solution, continue to stir for 30 minutes to form a uniform polymer emulsion. Ne...

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Abstract

The invention discloses a preparation method of open-celled high-energy molecular microspheres. The method comprises the following steps: dissolving a nitrocellulose-containing molecular material with high energy in ethyl acetate at room temperature, adding an alkane solvent under stirring, gradually adding an aqueous solution containing an emulsifier, fully emulsifying to obtain a polymer emulsion with the internal phase of alkane and the aqueous solution, carrying out secondary dispersion on the polymer emulsion in an aqueous solution containing a dispersant under stirring to form spherical droplets, adding water or an aqueous solution to the obtained system to make the spherical droplets formed by the polymer emulsion gradually hardened to form high-energy molecular particles, separating, and drying to obtain the open-celled high-energy molecular microspheres. The method has the advantages of short process flow, simple operation, controllable pore structure, safety and environmental protection, and is suitable for batch preparation of open-celled high-energy molecular spheres with the aperture of micrometer or submicron and the particle size of less than 100[mu]m.

Description

Technical field [0001] The invention belongs to the technical field of energetic composite materials, in particular to a method for preparing energetic polymer microspheres with an open-pore structure. Background technique [0002] Energetic polymer microspheres are one of the necessary ingredients for the manufacture of high-performance propellants. The size of energetic polymer microspheres directly affects the molding processability of the propellant and the uniformity of material mixing. Usually, the particle size of the energetic polymer microspheres is mostly 1-100 microns. The typical energetic polymer microspheres are nitrocellulose microspheres. [0003] US Patent US3639183 discloses a method for preparing plasticized nitrocellulose or cellulose acetate. The typical process is to use nitromethane to dissolve cellulose acetate into a varnish-like sol, and then add petroleum sulfonic acid emulsifier and water to the sol system In the process, the materials are transferred ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02
CPCB01J13/02
Inventor 蔺向阳王萍
Owner NANJING UNIV OF SCI & TECH
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