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Method for obtaining solid particles from water solution by utilizing supercritical carbon dioxide

A technology of carbon dioxide and solid particles, which is applied in the direction of liquid separation into beads and granulation, and can solve problems such as high operating pressure and operating temperature

Inactive Publication Date: 2010-06-02
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above-mentioned supercritical fluid technologies can be used to treat aqueous systems to obtain solid particles, and are already in the stage of industrialization, these methods all require higher operating pressure (such as SEDS) or operating temperature (such as CAN ~ BD and SAA)

Method used

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  • Method for obtaining solid particles from water solution by utilizing supercritical carbon dioxide
  • Method for obtaining solid particles from water solution by utilizing supercritical carbon dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: From SiO 2 Obtaining Submicron SiO from Colloidal Sol 2 particles.

[0027] The medicaments used are: tetraethyl orthosilicate TEOS (Sinopharm Group Chemical Reagent Co., Ltd.), absolute ethanol (Sinopharm Group Chemical Reagent Co., Ltd.), glacial acetic acid (Sinopharm Group Chemical Reagent Co., Ltd.), CO 2 (Provided by Xiamen Tongan Carbon Dioxide Filling Station, purity ≥ 98%).

[0028] When preparing the proportioning ratio of sol raw materials TEOS: water: ethanol: acid=1: 6.4: 8: 0.085 (molar ratio), sol aging time 5h, solution flow rate is 2ml / min, pre-expansion temperature T 1 at 45°C, the diameter of the nozzle is 100μm, and the pressure after the nozzle is P 2 is 0.1MPa, and when the pre-expansion pressure P 1 Solid SiO obtained under 8MPa and 10MPa 2 The average particle diameters are 0.38 μm and 0.58 μm (serious particle aggregation at 17 MPa). It can be confirmed by infrared analysis that the obtained solid particles are SiO 2 .

Embodiment 2

[0029] Example 2: From SiO 2 Obtaining nano-SiO from sol 2 particles.

[0030] The agents used are: tetraethyl orthosilicate TEOS (Sinopharm Group Chemical Reagent Co., Ltd.), absolute ethanol (Sinopharm Group Chemical Reagent Co., Ltd.), ammonia water (Sinopharm Group Chemical Reagent Co., Ltd.), CO 2 (Provided by Xiamen Tongan Carbon Dioxide Filling Station, purity ≥ 98%).

[0031] When the proportioning TEOS of preparation sol raw material: water: ethanol: ammoniacal liquor=1: 5: 35.8: 1.25 (molar ratio), sol aging time 5h, solution flow rate is 2ml / min, pre-expansion temperature T 1 at 45°C, the diameter of the nozzle is 100μm, and the pressure after the nozzle is P 2 is 0.1MPa, and when the pre-expansion pressure P 1 Solid SiO obtained under 8MPa and 10MPa 2 The particle size is <100nm.

Embodiment 3

[0032] Example 3: Obtaining bovine serum albumin particles from aqueous solution.

[0033] The reagents used are: BSA (purchased from Xinglongda Pharmaceutical Co., Ltd. and Fujian Huacan Biotechnology Co., Ltd., Sanland~Chem International Inc. and Huagene Biosciences, LTD.); carbon dioxide (purity ≥ 98%, Xiamen Air Separation Special Gas Co., Ltd. company); absolute ethanol (Sinopharm Chemical Reagent Co., Ltd.).

[0034] (1) At the pre-expansion temperature T 1 50 ℃, 100m nozzle, BSA concentration 20mg / g, ethanol concentration 20% (mass percentage of ethanol in water), solution flow rate is 1ml / min, P 2 is 0.1MPa, and when the pre-expansion pressure P 1 The particles of BSA prepared under 8MPa and 10MPa are spherical, and the average particle diameters of solid BSA are 0.82μm and 0.73μm, respectively. Other conditions are the same as above, when P 2 1MPa, P 1 The particles of BSA prepared under 8 MPa are spherical, and the average particle diameter of solid BSA is 0.90 ...

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Abstract

A method for obtaining solid particles from water solution by utilizing supercritical carbon dioxide relates to a method for obtaining solid particles and composite solid particles with release control effect from water solution. The invention provides a device and a method for obtaining solid particles from water solution by utilizing supercritical carbon dioxide. A carbon dioxide conveying mechanism, a water solution conveying mechanism, a particle collecting and recycling mechanism and a control and display mechanism are arranged. Solution of a water-soluble material, an entrainer and wateris arranged in a high pressure system and then enters a passage of a two-way nozzle; carbon dioxide is conveyed into the other passage of the coaxial two-way nozzle so as to achieve a supercritical fluid state; the solution of the water-soluble material, the entrainer and the water is atomized; solid particles are collected in a particle collecting chamber after the atomization; the entrainer andthe water solution is taken away by the carbon dioxide; after cooling and separation, the entrainer and the carbon dioxide are recycled.

Description

technical field [0001] The invention relates to a method for obtaining solid particles and composite solid particles with controlled release effect from aqueous solution, in particular to a method for obtaining protein particles from aqueous solution by means of supercritical carbon dioxide atomization and entrainer as auxiliary means . A method and device for water-soluble inorganic or organic material particles and composite particles thereof. Background technique [0002] Obtaining solid particles or preparing composite solid particles (including microcapsules) from aqueous solution has always been an important field in the chemical, pharmaceutical, food and other industries. For substances that are biologically active, impact-sensitive, heat-sensitive, structurally unstable, and easily chemically decomposed, mild drying conditions are required, and toxic organic solvents, etc. should be avoided. Therefore, the spray-drying method used on a large scale in the industry ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J2/04
Inventor 李军熊开斌苏玉忠
Owner XIAMEN UNIV