CN1528505A - Crystallizing kettle for preparing superfine powder using supercritical anti-solvent process - Google Patents
Crystallizing kettle for preparing superfine powder using supercritical anti-solvent process Download PDFInfo
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- CN1528505A CN1528505A CNA200310104825XA CN200310104825A CN1528505A CN 1528505 A CN1528505 A CN 1528505A CN A200310104825X A CNA200310104825X A CN A200310104825XA CN 200310104825 A CN200310104825 A CN 200310104825A CN 1528505 A CN1528505 A CN 1528505A
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Abstract
The invention relates to a crystallizing kettle using the supercritical fluid desolvation course to prepare ultrafine powder, mainly composed of kettle body, material basket, inner and outer spray nozzles, etc. Its character: a penetrable straight spray hole is set on the cavity wall of the inner spray nozzle, and the outer surface of the inner spray nozzle and the inner surface of the outer spray nozzle form a supercritical fluid ringed channel, which gradually shrinks to become narrow to form a narrow and small spray hole. It can evenly disperse the solution into micro liquid drops in the supercritical fluid, so that the product has small grain size and uniformly distributed grains. It is applied to the field where the solvent in the solution can dissolve in the supercritical fluid but the solute in the solution does not dissolve in the supercritical fluid (or the solubility very small).
Description
Technical field
The invention belongs to the chemical machinery technical field, relate to a kind of equipment for preparing superfine powder, especially relate to a kind of design for preparing the crystallization kettle of superfine powder with the super-critical anti-solvent process.
Background technology
The method of utilizing supercritical fluid to prepare superfine powder has multiple at present, as supercritical solution rapid expanding method (being called for short RESS) and super-critical anti-solvent method methods such as (being called for short SAS), these methods respectively have its scope of application, and wherein the application prospect of SAS method is more extensive.The SAS ratio juris is: the solid material that will make superfine powder is dissolved in earlier as solute and forms solution in the organic solvent, in crystallization kettle, be sprayed onto this solution in the supercritical fluid rapidly again, because the solute in the solution is insoluble to supercritical fluid, but solvent can dissolve each other with supercritical fluid, like this supercritical fluid with the solvent in the solution anti-molten after, in the extremely short time, make solution form very big degree of supersaturation, impel solute to separate out with the form of nanometer or micron particles.On this method technology is feasible, can be for the crystallization kettle of suitability for industrialized production use but lack at present.Existing crystallization kettle only is applicable to experimental study, can not be used for the production of relatively large product, and shortcomings such as the particle diameter of the ultrafine dust of existence preparation is big, particle diameter skewness.
Summary of the invention
The objective of the invention is, provide a kind of and prepare the crystallization kettle of superfine powder with the super-critical anti-solvent process, this crystallization kettle has that output is big, the sufficient characteristics of gas-liquid mixed, thereby makes the particle diameter of superfine powder product of preparation little, particle diameter is evenly distributed.
Technical scheme of the present invention is as follows:
A kind ofly prepare the crystallization kettle of superfine powder with the super-critical anti-solvent process, this crystallization kettle mainly is made of kettle cover, kettle, charging basket, inner nozzle and outer nozzle etc.The invention is characterized in: inner nozzle is provided with solution cavity, is provided with the straight spray orifice of penetrability in the lower end of this chamber wall, and wall upper end in chamber is connected with kettle cover: the solution entrance hole is set on kettle cover, and the solution cavity of inner nozzle is connected with this solution entrance hole; Inner nozzle chamber wall and kettle cover junction are provided with potted component, so that after solution enters the nozzle solution cavity by the solution entrance hole on the kettle cover, can only flow out by the straight spray orifice on the wall of chamber; The outer nozzle upper end is connected with kettle cover, form a supercritical fluid annular channel between the inner surface of outer nozzle and the outer surface of inner nozzle, this annular channel upper end is connected with supercritical fluid entrance hole on the kettle cover, and the lower end is shunk gradually and narrowed down, and forms a narrow and small jet; Outer nozzle and kettle cover junction are provided with potted component, so that after supercritical fluid enters supercritical fluid circular passage between inner nozzle and the outer nozzle by the supercritical fluid entrance hole on the kettle cover, can only flow out by the narrow and small jet of outer nozzle lower end; The charging basket lower end is provided with microporous filter element, the upper end links to each other with outer nozzle and (also can link to each other with kettle cover, the two effect is identical), whole charging basket is placed in the kettle, the kettle lower end is provided with leadout hole, the upper end is connected with kettle cover, and is provided with potted component in this junction, prevents that mixture passes through this junction to external leakage in the kettle.
The solution that contains solute enters the inner nozzle solution cavity by the solution entrance hole on the kettle cover, and simultaneously supercritical fluid enters supercritical fluid annular channel between inner nozzle and the outer nozzle by the supercritical fluid entrance hole on the kettle cover.Because this supercritical fluid runner narrows down gradually, make flow the gradually speedup of supercritical fluid in this runner.When supercritical fluid is flowed through straight spray orifice on the wall of inner nozzle chamber, the solution in the inner nozzle solution cavity is taken out of by straight spray orifice, made solution disperse rapidly to become small droplet, and be sprayed in the charging basket by the jet of supercritical fluid annular channel lower end.In this process, the solvent in the solution droplet by supercritical fluid anti-molten after, in the extremely short time, formed very big degree of supersaturation, the solute in the solution droplet is separated out with the form of ultrafine dust.Formed homogeneous mixture behind the solvent in the anti-broad liquid of supercritical fluid in the charging basket is behind the microporous filter element by the charging basket lower end, by the leadout hole outflow of kettle lower end.Ultrafine dust in the charging basket is separated obstruct in charging basket by the microporous filter element of this charging basket lower end, becomes the superfine powder that will prepare.
For the above-described crystallization kettle for preparing superfine powder with the super-critical anti-solvent process, if required output is bigger, can increase kettle and charging basket diameter, correspondingly increase inner nozzle and outer nozzle diameter, increase the straight nozzle hole number on the wall of inner nozzle chamber, these straight spray orifices are even, axisymmetric to be arranged on the taper seat, radially.If required output is less, can suitably reduce kettle and charging basket diameter, reduce the straight nozzle hole number of inner nozzle chamber wall, up to a straight spray orifice, promptly adopt the inner nozzle of single straight spray orifice.When adopting the inner nozzle of single straight spray orifice, this straight spray orifice is arranged on the axis of symmetry of inner nozzle.
The present invention is best suited for solvent in the solution can be dissolved in the occasion that solute in supercritical fluid and the solution is insoluble to supercritical fluid (or solubility is very little).
Advantage of the present invention and effect are:
1. shrink the supercritical fluid annular channel that narrows down gradually owing to having adopted, supercritical fluid flowing in this runner quickened gradually, created good hydrodynamics and thermodynamic condition for being dispersed into mist droplet after solution is taken out of by straight spray orifice and making solution in the extremely short time, form very big degree of supersaturation from solution cavity, thereby made prepared superfine powder particle diameter little and be evenly distributed.
2. pass through to regulate the straight nozzle hole number of inner nozzle, and kettle and charging basket diameter, different requirements can be adapted to product yield.That is to say,, can adopt the inner nozzle of a plurality of straight spray orifices if desired than big output; Less if desired output can adopt the inner nozzle of single straight spray orifice.
Description of drawings
Accompanying drawing 1 is the structural representation of first kind of embodiment of the present invention.
Among the figure: 1 kettle cover; 2 annular outer nozzles; 3 inner nozzles; 4 solution entrance holes; 5 inner nozzle solution cavities; 7 entrance holes; 8 supercritical fluid annular channels; 10 bolts; 11 straight spray orifices; 12 jets; 6,9,13 is potted component; 14 kettlies; 15 charging baskets; 16 microporous filter elements; 17 leadout holes.
Accompanying drawing 2 is structural representations of second kind of embodiment of the present invention.
Among the figure: 1 kettle cover; 2 annular outer nozzles; 3 inner nozzles; 4 solution entrance holes; 5 inner nozzle solution cavities; 7 entrance holes; 8 supercritical fluid annular channels; 11 straight spray orifices; 12 jets; 6,9,13 is potted component; 14 kettlies; 15 charging baskets; 16 microporous filter elements; 17 leadout holes; 18 glands.
The specific embodiment
Be described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.
First kind of embodiment: adopt the inner nozzle of a plurality of straight spray orifices, being applicable to need more large-tonnage occasion.
Tubular inner nozzle 3 is provided with a cylindrical solution cavity 5 among Fig. 1, is provided with the straight spray orifice 11 of a plurality of penetrability in this wall lower end, chamber, and these straight spray orifices are distributed on the taper seat, radially evenly, axisymmetrically.Wall upper end in chamber is connected with kettle cover 1, and connected mode can adopt and be threaded, welding etc.Solution entrance hole 4 is set on kettle cover.The solution cavity 5 of inner nozzle 3 is connected with this solution entrance hole 4.The chamber wall of inner nozzle 3 is provided with potted component 6 (if the two adopts welding manner to be connected and can to guarantee the seal of welding, the sealing element can be set) with the junction of kettle cover 1, and the sealing element can be plain cushion, "O etc.Like this, after solution flows into inner nozzle solution cavity 5 by the solution entrance hole on the kettle cover 14, can only flow out by the straight spray orifice on the wall of chamber 11.The upper end of annular outer nozzle 2 is connected with kettle cover 1, and connected mode can adopt and be threaded, welding etc.Form a supercritical fluid annular channel 8 between the outer surface of the inner surface of outer nozzle 2 and inner nozzle 3.Kettle cover is provided with supercritical fluid entrance hole 7.The upper end of supercritical fluid annular channel 8 is connected with supercritical fluid entrance hole 7 on the kettle cover 1, and the lower end is shunk gradually and narrowed down, and forms a narrow and small jet 12.Outer nozzle 2 is provided with potted component 9 (if the two adopts welding manner to be connected, and can guarantee the sealing of welding, the sealing element can be set) with kettle cover 1 junction, and the sealing element can be plain cushion, " O " type ring etc.Like this, when supercritical fluid enters supercritical fluid circular passage 8 between inner nozzle 3 and the outer nozzle 2 by the supercritical fluid entrance hole 7 on the kettle cover 1 after, can only flow out by the narrow and small jet 12 of outer nozzle 2 lower ends.The lower end of charging basket 15 is provided with a microporous filter element 16, and this microporous filter element can be stainless steel sintering filter element, filter membrane, silk screen etc., intercepts in charging basket 15 as long as can separate formed superfine powder.The upper end of charging basket 15 links to each other with outer nozzle 2, and connected mode can adopt and be threaded, articulate etc.Whole charging basket 15 is placed in the kettle 14.Kettle 14 lower ends are provided with leadout hole 17, and the upper end is connected with kettle cover 1 flange, and are fixing with bolt 10.Modes such as kettle 14 can also adopt with being connected of kettle cover 1 and be threaded, clamp connection, gland connection.Junction at kettle 14 and kettle cover 1 is provided with potted component 13, and the sealing element can be "O, Polyurethane sealing ring, plain cushion etc.Like this, just can prevent that the junction of mixture in the kettle (superfine powder product, solvent and supercritical fluid after dissolving each other) by kettle 14 and kettle cover 1 is to external leakage.
The solution that contains solute enters inner nozzle solution cavity 5 by the solution entrance hole 4 on the kettle cover 1, and simultaneously supercritical fluid enters the supercritical fluid circular passage 8 of 2 at inner nozzle 3 and outer nozzle by the supercritical fluid entrance hole 7 on the kettle cover 1.Because supercritical fluid circular passage 8 narrows down gradually, make flow the gradually speedup of supercritical fluid in this runner.When supercritical fluid is flowed through straight spray orifice 11 on the wall of inner nozzle chamber, solution in the inner nozzle solution cavity 5 is taken out of by this straight spray orifice 11, make solution be dispersed into mist droplet rapidly, and be sprayed in the charging basket 15 by the jet 12 of 8 lower ends, supercritical fluid circular passage.In this process, the solvent in the solution droplet by supercritical fluid anti-molten after, in the extremely short time, formed very big degree of supersaturation, the solute in the solution droplet is separated out with the form of ultrafine dust.Form homogeneous mixture behind the solvent in the anti-broad liquid of supercritical fluid in the charging basket 15, behind the microporous filter element 16 by charging basket 15 lower ends, by leadout hole 1 outflow of kettle 14 lower ends.Ultrafine dust in the charging basket is separated obstruct in charging basket 15 by the microporous filter element 16 of charging basket 15 lower ends, becomes the superfine powder product that will prepare.
Second kind of embodiment: adopt the inner nozzle of single straight spray orifice, be applicable to the occasion that needs less output.
Straight spray orifice 11 on the inner nozzle chamber wall among Fig. 2 is arranged on the axis of inner nozzle 3.The gland connected mode is adopted in being connected of kettle 14 and 1 of kettle cover, promptly with a gland 18 kettle cover 1 is fixed on the position that is connected with kettle 14, adopts between gland 18 and the kettle 14 to be threaded.Part among Fig. 1 of the structure of each part of all the other among Fig. 2, function etc. and same numeral is identical.
Claims (3)
1. one kind prepares the crystallization kettle of superfine powder with the supercritical fluid anti-solvent process, and this crystallization kettle mainly is made up of kettle cover, kettle, charging basket, inner nozzle and outer nozzle etc.; It is characterized in that:
1) inner nozzle is provided with solution cavity, in this wall lower end, chamber the straight spray orifice of penetrability is set, and wall upper end in chamber is connected with kettle cover, and is provided with potted component in this junction;
2) the solution entrance hole is set on kettle cover, the solution cavity of inner nozzle is connected with this solution entrance hole, the outer nozzle upper end is connected with kettle cover, and at this place of connecing potted component is set, and forms a supercritical fluid annular channel between the inner surface of outer nozzle and the outer surface of inner nozzle;
3) the supercritical fluid entrance hole is set on kettle cover, the upper end of supercritical fluid annular channel is connected with this supercritical fluid entrance hole, and the lower end is shunk gradually and narrowed down, and forms a narrow and small spout;
4) the charging basket lower end is provided with microporous filter element, and the upper end is connected with outer nozzle or kettle cover, and whole charging basket is placed in the kettle;
5) the kettle lower end is provided with leadout hole, and the upper end is connected with kettle cover, and in this junction potted component is set.
2. prepare the crystallization kettle of superfine powder according to claim 1 is described with the supercritical fluid anti-solvent process, it is characterized in that: a plurality of straight spray orifices are set on the inner nozzle, and these straight spray orifices are distributed on the taper seat radial evenly, axisymmetrically.
3. prepare the crystallization kettle of superfine powder according to claim 1 is described with the supercritical fluid anti-solvent process, it is characterized in that: a straight spray orifice is set on the wall of inner nozzle chamber, and this straight spray orifice is arranged on the axis of symmetry of inner nozzle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310104825 CN1238101C (en) | 2003-10-10 | 2003-10-10 | Crystallizing kettle for preparing superfine powder using supercritical anti-solvent process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310104825 CN1238101C (en) | 2003-10-10 | 2003-10-10 | Crystallizing kettle for preparing superfine powder using supercritical anti-solvent process |
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| CN1528505A true CN1528505A (en) | 2004-09-15 |
| CN1238101C CN1238101C (en) | 2006-01-25 |
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| CN 200310104825 Expired - Fee Related CN1238101C (en) | 2003-10-10 | 2003-10-10 | Crystallizing kettle for preparing superfine powder using supercritical anti-solvent process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7175886B2 (en) * | 2001-02-26 | 2007-02-13 | Dompe' Pha.R.Ma S.P.A. | Apparatus and method for micron and submicron particle formation |
| CN100352558C (en) * | 2005-03-04 | 2007-12-05 | 山东大学 | Nozzle for micro and nano material preparation by interior mixing supercritical fluid |
| CN100352559C (en) * | 2005-03-04 | 2007-12-05 | 山东大学 | Nozzle for micro and nano material preparation by exterior mixing supercritical fluid |
| CN106563286A (en) * | 2016-11-03 | 2017-04-19 | 中北大学 | Crystallization hanging basket used for preparing nanometer and micrometer particles through supercritical atomization and crystallization process |
| CN106563399A (en) * | 2016-11-18 | 2017-04-19 | 中北大学 | Method for preparing nano microcapsule of shell-core structure from supercritical fluid |
-
2003
- 2003-10-10 CN CN 200310104825 patent/CN1238101C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7175886B2 (en) * | 2001-02-26 | 2007-02-13 | Dompe' Pha.R.Ma S.P.A. | Apparatus and method for micron and submicron particle formation |
| US7635442B2 (en) | 2001-02-26 | 2009-12-22 | Dompe Pha.R.Ma S.P.A. | Apparatus and method for micron and submicron particle formation |
| CN100352558C (en) * | 2005-03-04 | 2007-12-05 | 山东大学 | Nozzle for micro and nano material preparation by interior mixing supercritical fluid |
| CN100352559C (en) * | 2005-03-04 | 2007-12-05 | 山东大学 | Nozzle for micro and nano material preparation by exterior mixing supercritical fluid |
| CN106563286A (en) * | 2016-11-03 | 2017-04-19 | 中北大学 | Crystallization hanging basket used for preparing nanometer and micrometer particles through supercritical atomization and crystallization process |
| CN106563286B (en) * | 2016-11-03 | 2019-04-05 | 中北大学 | A kind of overcritical atomization crystallization processes preparation receives micron particles and crystallizes hanging basket |
| CN106563399A (en) * | 2016-11-18 | 2017-04-19 | 中北大学 | Method for preparing nano microcapsule of shell-core structure from supercritical fluid |
| CN106563399B (en) * | 2016-11-18 | 2019-07-09 | 中北大学 | A kind of method that supercritical fluid prepares " shell-core " structure nano microcapsules |
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| Publication number | Publication date |
|---|---|
| CN1238101C (en) | 2006-01-25 |
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