CN1498675A - Method and device for producing ultramicron by using supercritical gas saturation solution - Google Patents
Method and device for producing ultramicron by using supercritical gas saturation solution Download PDFInfo
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- CN1498675A CN1498675A CNA02146099XA CN02146099A CN1498675A CN 1498675 A CN1498675 A CN 1498675A CN A02146099X A CNA02146099X A CN A02146099XA CN 02146099 A CN02146099 A CN 02146099A CN 1498675 A CN1498675 A CN 1498675A
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- ultrafine dust
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- saturated solution
- carbon dioxide
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Abstract
A process and system for preparing the superfine microparticles from the supercritical gas saturated solution is disclosed, which features that it is suitable for the solute dissolved in water other than CO2 and organic solvent. It has wide application fields, especially for preparing protein, polypeptide, nucleic acid, or gene materials.
Description
Technical field
The present invention relates to a kind of manufacturing technology of ultrafine dust, particularly relate to a kind of method and apparatus of making ultrafine dust with the supercritical gas saturated solution.
Background technology
Now the The characteristics with various manufacturing ultrafine dust methods is as follows: (seeing Table 1)
| Method | Granularity | Size distribution | Dissolvent residual | To heat-sensitive substance | Industrialization |
| Spray-drying | Little | Narrower | Have | Improper | Suitable |
| Freeze drying | Less | Wide | Do not have | Suitable | Suitable |
| Chemical method | Little | Narrow | Have | Suitable | Improper |
| Fluid jet | Little | Wide | Do not have | Improper | Suitable |
| Supercritical methanol technology | Little | Narrow | ????* | Suitable | ??* |
*Variant according to the method difference.
Method and methods such as spray-drying, freeze drying, jet pulverizing and chemistry that supercritical fluid is made ultrafine dust compare, and have certain characteristic, are specially adapted to the processing of the ultrafine dust of medicine biochemistry, organic material.In fact supercritical process manufacturing ultrafine dust comprises several different methods, finally be divided into two kinds of methods, be fast expanding supercritical solution (Rapid ExpansionSupercritical Solutions, be called for short RESS) and supercritical back extractant (SupercriticalAntiSolvent is called for short SAS) method (seeing Table 2).
Two kinds of overcritical manufacturing ultrafine dust methods relatively
| Project | ????RESS | ????SAS |
| Particle diameter | 0.01-5 micron | 0.1-5 micron |
| Particle diameter distributes | Narrow | Narrow |
| The mode of production | Continuously | The gap |
| Output | Greatly | Depend on the still capacity |
| Dissolvent residual | Do not have | Have |
| Equipment investment | In | Greatly |
| Range of application | Little | Greatly |
Annotate: RESS is the fast expanding supercritical solution method, it is applied to process the solute that carbon dioxide can dissolve, principle is that solution is dissolved in solute in the carbon dioxide because rapid expanding and absorbing and cooling temperature in the fast spraying process, and solubility reduces, and the solute precipitating forms particulate; But SAS is the supercritical back extractant method, is to utilize carbon dioxide not dissolve the solute that can dissolve each other with organic solvent.Do the time spent when solution and carbon dioxide, solvent and carbon dioxide in the solution dissolve each other, and the solubility of solute in solvent reduces and precipitating, forms particulate.
Above-mentioned two kinds of methods, RESS can only be used to process the solute that is dissolved in carbon dioxide; SAS then processes the solute that is dissolved in organic solvent.These two kinds of methods can not realize being used to process water-soluble solute, especially can not be implemented in the special application in amino acid, protein, polypeptide, nucleic acid and gene field of biochemical medicine.
Summary of the invention
The objective of the invention is to overcome the above-mentioned deficiency of prior art, a kind of method with supercritical gas saturated solution manufacturing ultrafine dust is provided, this method is applicable to the water-soluble solute of processing.
The object of the present invention is to provide the equipment that is used to implement this method.
For achieving the above object, the present invention makes the method for ultrafine dust with the supercritical gas saturated solution, it comprises that RESS is that fast expanding supercritical solution method and SAS are the supercritical back extractant method, its granulation step is the solution with water dissolved substances (solute), after carbon dioxide is saturated, in uniform temperature, under pressure and the flow condition, after the current limiter rapid expanding, at this moment solution is atomized into very fine aerosol, be carried to the warm area of uniform temperature again through assist gas, at this moment carbon dioxide in the aerosol and water volatilize and are discharged with auxiliary gas, promptly obtain ultrafine dust.
As optimization, described auxiliary gas can be nitrogen, argon gas or air.
Be preferably nitrogen as optimizing described auxiliary gas.
Be used to realize that the present invention makes the equipment of ultrafine dust method with the supercritical gas saturated solution, it comprises the collection still, at this current limiter threeway very little with the dead volume that is connected current limiter arranged above the collection still, the other two ends of threeway are connected with solution line with carbon dioxide respectively, and this collection still is provided with the pipeline that connects auxiliary gas simultaneously.
As optimization, described threeway is the stainless steel threeway of dead volume less than 1 microlitre.
As optimization, described capillary is an internal diameter less than 100 microns quartz capillary.
After adopting above-mentioned technical solution, because the present invention is with water as solvent, its applied range, be applicable to biochemical medicine, various binding agent, various metal oxide, plastic coating, plastic additive, superconductor and spinelle, be particularly useful for the processing of the ultrafine dust of protein, polypeptide, nucleic acid, gene, its particle diameter is little, narrow particle size distribution, no solvent residue, and equipment is simple, production cost is low.
The specific embodiment
Be described further the method that supercritical gas saturated solution of the present invention is made ultrafine dust below in conjunction with instantiation, comprise that RESS is the fast expanding supercritical solution method, SAS supercritical back extractant method, its step is the solute that the water dissolving needs pulverizing, after carbon dioxide is saturated, in uniform temperature, under pressure and the liquid inventory condition, after the current limiter rapid expanding, at this moment solution is atomized into very fine aerosol, be carried to the warm area of uniform temperature again through auxiliary gas, at this moment carbon dioxide in the aerosol and water expand and volatilization is discharged with auxiliary gas, promptly obtain ultrafine dust.
Embodiment 1
Specifically be that the concentration of alanine (amino acid whose a kind of) by 0.5% that will pulverize earlier prepares and puts into container 7, again the heat exchangers 11 before the current limiter 10 be heated to 60 ℃, presetting the temperature of collecting still 3 simultaneously is 35 ℃, opens carbon dioxide air source valve V
1With the power supply that starts molding machine 2, at this moment pressure carbon dioxide is adjusted to 10MPa, opens constant-flux pump 6 and V again
3Valve is opened valve V simultaneously
2, at this moment the solution in the NaOH solution tank NaOH 7 generates aerosol in dead volume very little threeway and carbon dioxide junction, and aerosol contacts with the auxiliary gas of opening in advance (being generally nitrogen) at collection still place through current limiter, behind 35-40 ℃ warm area, again by filter 5, V
5Valve is to mass flowmenter 9 discharging carbon dioxide and water, and ultrafine dust is then stayed and collected in the still.
Embodiment 2
Specifically be that the concentration of the sodium chloride that will pulverize earlier (promptly 1%) by 0.2% prepares and puts into container 7, again the heat exchangers 11 before the current limiter 10 be heated to 80 ℃, presetting the temperature of collecting still 3 simultaneously is 60 ℃, opens carbon dioxide air source valve V
1With the power supply that starts molding machine 2, at this moment pressure carbon dioxide is adjusted to 10MPa, opens constant-flux pump 6 and V again
3Valve is opened valve V simultaneously
2, at this moment the solution in the NaOH solution tank NaOH 7 generates aerosol in dead volume very little threeway and carbon dioxide junction, and aerosol contacts with the auxiliary gas of opening in advance (being generally nitrogen) at collection still place through current limiter, behind 60 ℃ warm area, again by filter 5, V
5Valve is to mass flowmenter 9 discharging carbon dioxide and water, and ultrafine dust is then stayed and collected in the still.
The equipment that is used to implement above-mentioned manufacturing ultrafine dust method comprises the collection still, be provided with current limiter and the threeway that is connected with current limiter above the collection still at this, the other two ends of threeway are connected with solution line with carbon dioxide respectively, collect the connecting pipe that still is provided with auxiliary gas simultaneously.
Make the equipment of ultrafine dust method and be described further being used to implement supercritical gas saturated solution of the present invention below in conjunction with accompanying drawing, this equipment comprises carbon dioxide steel cylinder 1, molding machine 2, heat exchanger 11, threeway 4, collects still 3, filter 5, constant-flux pump 6, NaOH solution tank NaOH 7, auxiliary gas cylinder 8, mass flowmenter 9, current limiter 10, also comprise valve V
1, V
2, V
3, V
4, V
5
Threeway 4 described in this equipment is the stainless steel threeway of a dead volume less than 1 microlitre; Described current limiter is an internal diameter less than 100 microns quartz capillary.
Claims (6)
1, a kind of supercritical gas saturated solution is made the method for ultrafine dust, and it comprises that RESS is that fast expanding supercritical solution method, SAS are the supercritical back extractant method; It is characterized in that its granulation step is the solution with water dissolved substances (solute), after carbon dioxide is saturated under uniform temperature, pressure and liquid inventory condition, through the current limiter rapid expanding, at this moment solution is atomized into very fine aerosol, be carried to the warm area of uniform temperature again through auxiliary gas, at this moment carbon dioxide in the aerosol and water expand and volatilization is discharged with auxiliary gas, promptly get ultrafine dust.
2, supercritical gas saturated solution according to claim 1 is made the method for ultrafine dust, it is characterized in that described auxiliary gas is nitrogen.
3, supercritical gas saturated solution according to claim 1 is made the method for ultrafine dust, it is characterized in that described auxiliary gas is argon gas or air.
4, be used to implement the equipment that supercritical gas saturated solution of the present invention is made the method for ultrafine dust, it is characterized in that collecting and be provided with the current limiter threeway very little above the still with the dead volume that is connected with current limiter, the other two ends of threeway are connected with solution line with carbon dioxide respectively, collect still simultaneously and are provided with auxiliary gas connecting pipe.
5, be used to implement the equipment that supercritical gas saturated solution liquid of the present invention is made the method for ultrafine dust according to claim 4 is described, it is characterized in that described threeway is the stainless steel threeway of a dead volume less than 1 microlitre.
6, according to claim 4ly be used to implement the equipment that supercritical gas saturated solution of the present invention is made ultrafine dust, it is characterized in that described current limiter is an internal diameter less than 100 microns quartz capillary.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA02146099XA CN1498675A (en) | 2002-11-06 | 2002-11-06 | Method and device for producing ultramicron by using supercritical gas saturation solution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA02146099XA CN1498675A (en) | 2002-11-06 | 2002-11-06 | Method and device for producing ultramicron by using supercritical gas saturation solution |
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| CN1498675A true CN1498675A (en) | 2004-05-26 |
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| CNA02146099XA Pending CN1498675A (en) | 2002-11-06 | 2002-11-06 | Method and device for producing ultramicron by using supercritical gas saturation solution |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1302766C (en) * | 2005-06-23 | 2007-03-07 | 同济大学 | Method for preparing biological degradable polymer drug-carried fine particle by supercritical anti-solvent process |
| CN101778659B (en) * | 2007-06-20 | 2012-11-07 | 龙树能源私人有限公司 | Process for recovering products from fermentation |
| CN104764636A (en) * | 2014-12-04 | 2015-07-08 | 青岛科技大学 | Method for preparing PM2.5 aerosol based on gas saturated solution process |
| CN112978841A (en) * | 2021-03-05 | 2021-06-18 | 郑州大学 | Modular multistage-region mineralizing, metallurgy pressurizing and mineralizing system |
-
2002
- 2002-11-06 CN CNA02146099XA patent/CN1498675A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1302766C (en) * | 2005-06-23 | 2007-03-07 | 同济大学 | Method for preparing biological degradable polymer drug-carried fine particle by supercritical anti-solvent process |
| CN101778659B (en) * | 2007-06-20 | 2012-11-07 | 龙树能源私人有限公司 | Process for recovering products from fermentation |
| CN104764636A (en) * | 2014-12-04 | 2015-07-08 | 青岛科技大学 | Method for preparing PM2.5 aerosol based on gas saturated solution process |
| CN112978841A (en) * | 2021-03-05 | 2021-06-18 | 郑州大学 | Modular multistage-region mineralizing, metallurgy pressurizing and mineralizing system |
| CN112978841B (en) * | 2021-03-05 | 2023-10-17 | 郑州大学 | Modularized multistage area mineralization metallurgy pressurization mineralization system |
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