Method for preparing nano microcapsule of shell-core structure from supercritical fluid

A nano-microcapsule and supercritical flow technology, which is applied in microcapsule preparation, microsphere preparation, bulk chemical production, etc., can solve the problems of complex operation process, wide particle size distribution range, large coating particle size, etc., and achieve simple operation. , Narrow particle size distribution, easy to control effect

Inactive Publication Date: 2017-04-19
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problems of uneven coating, very large coating particle size, wide particle size distribution range, complicated operation process, limited application and pollution in the existing meth

Method used

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  • Method for preparing nano microcapsule of shell-core structure from supercritical fluid
  • Method for preparing nano microcapsule of shell-core structure from supercritical fluid
  • Method for preparing nano microcapsule of shell-core structure from supercritical fluid

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Embodiment 1

[0035] In this embodiment, a method for preparing nano-microcapsules with a "shell-core" structure with a supercritical fluid comprises the following steps:

[0036] 1) Combine 5g of RDX and Viton (F 26 ) 0.15g was added to dimethylformamide (DMF) 100mL and stirred until RDX was completely dissolved in DMF, F 26 Completely swell in DMF to form a solution, keep the temperature of the solution at 20°C;

[0037] 2) Turn on the temperature control switch of the supercritical atomization crystallization preparation system, set the temperature of the particle collection tank to 33°C, and set the initial supercritical CO 2 The temperature is 38 °C and preheated for 30 minutes.

[0038] 3) Set CO 2 The flow rate of the solution is 5kg / h, the flow rate of the solution is set at 2mL / min, and the working pressure of the particle collection tank is set at 8MPa.

[0039] 4) Turn on the CO 2 Cylinder valve, open CO 2 pump to make CO 2 Enter the supercritical atomization crystallizati...

Embodiment 2

[0046] In this embodiment, a method for preparing nano-microcapsules with a "shell-core" structure with a supercritical fluid comprises the following steps:

[0047] 1) Mix RDX (RDX) 15g and fluororubber (F 26 ) 0.45g was added to dimethylformamide (DMF) 100mL and stirred until RDX was completely dissolved in DMF, F 26 Completely swell in DMF to form a solution, keep the temperature of the solution at 25°C;

[0048] 2) Turn on the temperature control switch of the supercritical atomization crystallization preparation system, set the temperature of the particle collection tank to 36°C, and set the initial supercritical CO 2 The temperature is 50°C and preheated for 30 minutes.

[0049] 3) Set CO 2 The flow rate of the solution is 10kg / h, the flow rate of the solution is set at 2mL / min, and the working pressure of the particle collection tank is set at 13MPa.

[0050] 4) Turn on the CO 2 Cylinder valve, open CO 2 pump to make CO 2 Enter the supercritical atomization cryst...

Embodiment 3

[0055] In this embodiment, a method for preparing nano-microcapsules with a "shell-core" structure with a supercritical fluid comprises the following steps:

[0056] 1) Mix RDX (RDX) 30g and fluororubber (F 26 ) 0.9g was added to dimethylformamide (DMF) 100mL and stirred until RDX was completely dissolved in DMF, F 26 Completely swell in DMF to form a solution, keep the temperature of the solution at 30°C;

[0057] 2) Turn on the temperature control switch of the supercritical atomization crystallization preparation system, set the temperature of the particle collection tank to 40°C, and set the initial supercritical CO 2 The temperature is 65°C and preheated for 30 minutes.

[0058] 3) Set CO 2 The flow rate of the solution is 20kg / h, the flow rate of the solution is set at 2mL / min, and the working pressure of the particle collection tank is set at 18MPa.

[0059] 4) Turn on the CO 2 Cylinder valve, open CO 2 pump to make CO 2 Enter the supercritical atomization crysta...

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Abstract

The invention relates to a preparation method of a nano microcapsule of an energetic material by using supercritical CO2 as an anti-solvent, an atomizing medium and a drying medium. A series of problems that the cladding is not uniform, cladding particle sizes are too large, the distribution range of the particle sizes is wide, the process operation is complicated, the application is limited, the environment is polluted, and the like, and which exist in an existing technical method in which the micronization is carried out first and then the cladding is carried out are mainly solved. According to the method, by using the supercritical CO2 as the anti-solvent, the atomizing medium and the drying medium, and based on the supercritical principle that the atomization is carried out first and then the crystallization is carried out, after a solution is atomized through a spray nozzle, a crystal nucleus is formed and grows inside a fog drop; a molecular chain of a cladding material collapses towards the interior of the fog drop; as the sum of the nucleation and growth times of a crystal is less than the collapsing time of the molecular chain, the crystalline particle of the energetic material is tightly enwrapped by the cladding material; and the nano microcapsule of the shell-core structure is formed. By using the method, a micronization technique and a cladding technique are integrated; a preparation process is accomplished at one fling; the subsequent treatment is not needed; the production efficiency is high; the preparation quality of the microcapsule is good; and the sphericity of the particle is good.

Description

technical field [0001] The invention relates to a method for preparing nano-microcapsules with a "shell-core" structure from a supercritical fluid, in particular to a method using supercritical CO 2 Preparation method of nano-microcapsules of energetic material as anti-solvent, atomization medium and drying medium. Background technique [0002] Solid propellants play a very important role in the development of aerospace and missiles. Most of the high-energy energetic materials contained in solid propellants (such as HMX, CL-20, LLM-105, etc.) have high energy but high mechanical sensitivity, which brings great challenges to the development, use, storage, and transportation of propellants. Here comes the problem of unsafety and poor compatibility between propellant components. Therefore, high energy, low vulnerability, and insensitivity of energetic materials are one of the main goals to be achieved by solid propellants. [0003] At present, there are three main methods to...

Claims

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Application Information

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IPC IPC(8): B01J13/02B01J13/22C06B25/34
CPCB01J13/02B01J13/22C06B25/34Y02P20/54
Inventor 蔡兴旺杨继华张景林李洪旭陶博文
Owner ZHONGBEI UNIV
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