CN1554463A - Basic process flow for preparing superfine powder using supercritical fluid reverse solvent process - Google Patents
Basic process flow for preparing superfine powder using supercritical fluid reverse solvent process Download PDFInfo
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- CN1554463A CN1554463A CNA2003101208672A CN200310120867A CN1554463A CN 1554463 A CN1554463 A CN 1554463A CN A2003101208672 A CNA2003101208672 A CN A2003101208672A CN 200310120867 A CN200310120867 A CN 200310120867A CN 1554463 A CN1554463 A CN 1554463A
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- 239000002904 solvent Substances 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000000843 powder Substances 0.000 title claims abstract description 26
- 239000012530 fluid Substances 0.000 title claims description 35
- 230000006837 decompression Effects 0.000 claims abstract description 5
- 239000012296 anti-solvent Substances 0.000 claims description 50
- 238000002425 crystallisation Methods 0.000 claims description 44
- 230000008025 crystallization Effects 0.000 claims description 44
- 238000001808 supercritical antisolvent technique Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 9
- 238000007630 basic procedure Methods 0.000 claims description 6
- 230000004907 flux Effects 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract 2
- 239000007787 solid Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000003595 mist Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The present invention relates to basic technological process of preparing superfine powder material. The main technological apparatus includes solvent storage tank, solvent pump, solvent tanks, solution heater, crystallizers, counter-solvent storage tank, counter-solvent pump, counter-solvent heater, decompression unit, separating tank, condenser, etc. The present invention features the solvent tanks and the crystallizers capable of being parallelly connected for periodical operation, and solvent and counter-solvent capable of being used circularly to form semi-continuous closed operation mode. The basic process can raise the operation efficiency, lower power consumption, eliminate waste in solvent and counter-solvent and apply to industrial production.
Description
Technical field
The invention belongs to field of chemical engineering, relate to a kind of typical process flow, particularly prepare the typical process flow of superfine powder, be used for the preparation of superfine powdery material with the supercritical fluid anti-solvent process.
Background technology
In recent years, people have developed some advanced supercritical fluid process and have been used for preparing superfine powder according to the characteristic of supercritical fluid.Wherein, most representative is the super-critical anti-solvent process.The principle of super-critical anti-solvent is: the solid solute that will make superfine powder is dissolved in a certain solvent and forms solution, be generally organic solvent, select a kind of supercritical fluid as anti-solvent, be generally carbon dioxide, solute in the general not solvent soln of this anti-solvent, but can dissolve each other with solvent, when anti-solvent contacts with solution, anti-solvent diffuses to this solution rapidly, liquor capacity is expanded rapidly, solute solubility in solvent descends greatly, forms very big degree of supersaturation in the extremely short time, impels the solute crystallization to separate out.The main feature of super-critical anti-solvent process is: because supercritical fluid " extraction " effect can be separated out the very high superfine powder of purity; Just can make solvent and anti-separated from solvent by simple decompression, its solvent and anti-solvent all can be recycled; The control operation condition, i.e. pressure, temperature, concentration, flow rate can be controlled form, size and the Size Distribution of the powder that forms, and can obtain the superfine powder of micron even nano level even size distribution.At present, the typical process flow for preparing superfine powder with the super-critical anti-solvent process is step, promptly takes single crystallization kettle and dissolving tank intermittently operated, solvent and as the supercritical fluid of anti-solvent cycling and reutilization scarcely.This flow operations efficient is low, energy consumption is big, and solvent and the waste of anti-solvent are serious, should not be used for industrial production.
Summary of the invention
The purpose of this invention is to provide and a kind ofly prepare the semi continuous typical process flow of superfine powder with the super-critical anti-solvent process, it can improve operating efficiency effectively, reduces energy consumption, eliminates the waste of solvent and anti-solvent, is applicable to suitability for industrialized production.
Technical scheme of the present invention is as follows:
A kind of semi continuous typical process flow for preparing superfine powder with the super-critical anti-solvent process.Capital equipment in this flow process comprises: solvent tank, solvent pump, dissolving tank, solution heater, crystallization kettle, anti-solvent tank, anti-solvent pump, anti-solvent heater, decompressor, knockout drum, condenser and valve etc.The solvent that is come out by solvent tank enters dissolving tank after boosting through solvent pump, fully contacts with solid solute in dissolving tank, forms to have certain density solution, and this solution enters crystallization kettle after solution heater is heated to uniform temperature.Simultaneously the anti-solvent in anti-solvent tank through anti-solvent pump pressurize, the intensification of anti-solvent heater reaches certain pressure and temperature, enter crystallization kettle after becoming supercritical fluid.In crystallization kettle, having certain density solution is evenly distributed in the supercritical fluid with the form of mist droplet, supercritical fluid is anti-molten with the solvent in the solution rapidly, make this solution in the extremely short time, form very big degree of supersaturation, solute is wherein just separated out with the form of ultrafine dust, form the superfine powder product, and the supercritical fluid that is dissolved with solvent comes out to enter knockout drum after the decompressor decompression from crystallization kettle., after supercritical fluid and the separated from solvent, form anti-solvent of gas and liquid flux here, the inlet that liquid flux turns back to solvent pump recycles, and the anti-solvent of gas is after condenser condenses becomes the anti-solvent of liquid, and the inlet that is back to anti-solvent pump recycles.The invention is characterized in that be provided with two crystallization kettles and two dissolving tanks in this flow process, these two crystallization kettles, two dissolving tanks are in blocked operation in parallel respectively.Promptly when one of them crystallization kettle was in mode of operation, another crystallization kettle was in the discharging state, promptly unloaded the superfine powder Product Status; When one of them solvent tank was in mode of operation, another solvent tank was in state of charge, immediate shipment solid solute state.For each crystallization kettle and solvent tank, be by periodic intermittent mode operation, but whole flow process is continuous like this.Therefore, this basic procedure is called the semi continuous typical process flow.
The above-mentioned typical process flow for preparing superfine powder with the super-critical anti-solvent process, the entrance and exit that it is characterized in that being arranged on the dissolving tank of two blocked operations in parallel between solvent pump and the heater is connected in parallel respectively, forms inlet and contact and outlet and contact.Inlet and contact are communicated with the solvent pump outlet, and outlet and contact are communicated with the solvent heater inlet.Be respectively arranged with valve between these two solvent tank inlets and inlet and contact, outlet also is respectively arranged with valve with outlet and contact.The solution inlet and the supercritical fluid inlet that are arranged on the crystallization kettle of two blocked operations in parallel between solvent heater and anti-solvent heater and the decompressor are connected in parallel respectively, form solution inlet and contact and supercritical fluid inlet and contact.Solution inlet and contact are communicated with the solution heater outlet, and supercritical fluid inlet and contact are communicated with anti-solvent heater.Be respectively arranged with valve between the solution inlet of these two crystallization kettles and solution inlet and contact, also be respectively arranged with valve between supercritical fluid inlet and supercritical fluid inlet and contact.The outlet of these two crystallization kettles is connected in parallel respectively, forms outlet and contact.Outlet and contact are communicated with the decompressor inlet.Be respectively arranged with valve between the outlet of these two crystallization kettles and outlet and contact.
Above-mentioned prepare the typical process flow of superfine powder, it is characterized in that between each equipment, can setting up measurement, control instrument and valve etc., thereby strengthen measurement, the control effect of this basic procedure with the super-critical anti-solvent process.Valve in this basic procedure can be manual, also can be that this depends primarily on desired automaticity automatically.This basic procedure has been determined to face the essential characteristic that anti-dissolving agent process prepares superfine product with super, on the basis of this basic procedure, sets up other necessary equipment, can form the kinds of processes flow process.
Advantage of the present invention and effect are: owing to taked crystallization kettle and dissolving tank alternate modes of operation in parallel respectively, in addition whole flow process is continuous, " locked in " operation, solvent and anti-solvent all can Recyclings, thereby improved operating efficiency, reduce energy consumption, eliminated the waste of solvent and anti-solvent.This typical process flow is applicable to suitability for industrialized production.
The present invention is best suited for the solid solute that will make superfine powder can be dissolved in solvent, but insoluble or be slightly soluble in the occasion of anti-solvent.
Description of drawings
Fig. 1 is an example for preparing the superfine powder typical process flow with the super-critical anti-solvent process.
Among the figure: 1 is solvent tank, 3 is solvent pump, and 6 and 7 is dissolving tank, and 10 is solution heater, 13 and 14 is crystallization kettle, 15 is anti-solvent tank, and 17 is anti-solvent pump, and 18 is anti-solvent heater, 23 is decompressor, 24 is knockout drum, and 25 is condenser, and 2,4,5,8,9,11,12,16,19,20,21,22 is valve.
The specific embodiment
Be described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.
Prepare in the superfine powder typical process flow with the super-critical anti-solvent process, after solvent in solvent tank 1 boosts through solvent pump 3, enter dissolving tank 6 or 7, in dissolving tank 6 or 7, fully contact with solid solute, formation has certain density solution, this solution enters crystallization kettle 13 or 14 after solution heater 10 is heated to uniform temperature.Simultaneously the anti-solvent in anti-solvent tank heats up, reaches certain pressure and temperature, enters crystallization kettle 13 or 14 after becoming supercritical fluid through anti-solvent pump 17 and 18 pressurizations of anti-solvent heater.In crystallization kettle 13 or 14, having certain density solution is evenly dispersed in the supercritical fluid with the form of mist droplet, supercritical fluid is promptly anti-molten with the solvent in the solution, make this solution form very big saturation degree in the extremely short time, solute is wherein just separated out with the form of ultra-fine grain.The solute of separating out is filtered element and intercepts to become the superfine powder product in crystallization kettle, and the supercritical fluid that is dissolved with solvent comes out to enter knockout drum 24 after decompressor 23 decompressions through crystallization kettle.After supercritical fluid and the separated from solvent, form anti-solvent of gas and liquid flux here.The inlet that liquid flux is back to solvent pump 3 recycles, and the anti-solvent of gas is after condenser 25 is condensed into liquid, and the inlet that is back to anti-solvent pump 17 recycles.The invention is characterized in, be arranged on the dissolving tank 6 of two blocked operations in parallel between solvent pump 3 and the solvent heater 10 and 7 entrance and exit and be connected in parallel respectively, form inlet and contact 26 and outlet and contact 27.Inlet and contact 26 are communicated with the outlet of solvent pump 3, and outlet and contact 27 are communicated with solvent heater 10 inlets.These two solvent tank inlets and inlet and 26 of contacts are respectively arranged with valve 4 and 5, and outlet also is provided with respectively with outlet and contact 27 has valve 8 and 9.Like this, open valve 4 and 8, valve-off 5 and 9, (ie in solution is with after solid solute in the dissolving tank 6 fully contacts just can to make dissolving tank 6 be in mode of operation, formation has certain density solution), dissolving tank 7 is in loading operation state (replenishing new solid solute promptly for dissolving tank 7), thereby realizes the periodically mode of operation of blocked operation in parallel of two dissolving tanks.Be arranged on the crystallization kettle 13 of two blocked operations in parallel between solvent heater 10 and anti-solvent heater 18 and the decompressor 23 and 14 solution population and supercritical fluid inlet and be connected in parallel respectively, form solution inlet and contact 28 and supercritical fluid inlet and contact 29.Solution inlet and contact 28 are communicated with solution heater 10 outlets, and overcritical inlet and contact 29 are communicated with anti-solvent heater 18 outlets.The outlet of these two crystallization kettles is connected in parallel respectively, forms outlet and contact 30.Outlet and contact 30 are communicated with decompressor 23 inlets.The outlet of these two crystallization kettles and outlet and 30 of contacts are respectively arranged with valve 21 and 22.Like this, open valve 11,19 and 21, valve-off 12,20 and 22, just can make crystallization kettle 13 be in mode of operation, promptly in crystallization kettle 13, having certain density solution is evenly dispersed in the supercritical fluid with the form of mist droplet, supercritical fluid is promptly anti-molten with the solvent in the solution, make this solution in the extremely short time, form very big degree of supersaturation, solute is wherein just separated out and is formed the superfine powder product, and the supercritical fluid that is dissolved with solvent flows out from the crystallization kettle outlet, and crystallization kettle 14 is in the discharging mode of operation, be the new superfine powder product that forms of removal, thereby realize the periodically mode of operation of blocked operation in parallel of two crystallization kettles.
Claims (3)
1. prepare the typical process flow of superfine powder with the supercritical fluid anti-solvent process, the capital equipment in this flow process comprises: solvent tank, solvent pump, dissolving tank, solution heater, crystallization kettle, anti-solvent tank, anti-solvent pump, anti-solvent heater, decompressor, knockout drum, condenser and valve; The solvent that comes out from solvent tank enters dissolving tank after boosting through solvent pump, forms to have certain density solution in dissolving tank, and this solution enters crystallization kettle after solution heater is heated to uniform temperature; Simultaneously the anti-solvent that comes out from anti-solvent tank through anti-solvent pump pressurize, anti-solvent heater heats up and reaches certain pressure and temperature, enters crystallization kettle after becoming supercritical fluid; In crystallization kettle, supercritical fluid with the solvent in the solution anti-molten after, solute wherein forms the superfine powder product, and the supercritical fluid that is dissolved with solvent comes out to enter knockout drum after the decompressor decompression from crystallization kettle; , after supercritical fluid and the separated from solvent, form anti-solvent of gas and liquid flux here, the inlet that liquid flux turns back to solvent pump recycles, and the anti-solvent of gas is after condenser condenses becomes the anti-solvent of liquid, and the inlet that is back to anti-solvent pump recycles; It is characterized in that be provided with two crystallization kettles and two dissolving tanks in this flow process, these two crystallization kettles, two dissolving tanks are in blocked operation in parallel respectively; Promptly when one of them crystallization kettle was in mode of operation, another crystallization kettle was in the discharging state; When one of them solvent tank was in mode of operation, another solvent tank was in state of charge.
2. the typical process flow for preparing superfine powder with the supercritical fluid anti-solvent process according to claim 1, it is characterized in that, the entrance and exit that is arranged on the dissolving tank of two blocked operations in parallel between solvent pump and the heater is connected in parallel respectively, forms inlet and contact and outlet and contact; Inlet and contact are communicated with the solvent pump outlet, and outlet and contact are communicated with the solvent heater inlet; Be respectively arranged with valve between these two solvent tank inlets and inlet and contact, outlet also is respectively arranged with valve with outlet and contact; The solution inlet and the supercritical fluid inlet that are arranged on the crystallization kettle of two blocked operations in parallel between solvent heater and anti-solvent heater and the decompressor are connected in parallel respectively, form solution inlet and contact and supercritical fluid inlet and contact; Solution inlet and contact are communicated with the solution heater outlet, and supercritical fluid inlet and contact are communicated with anti-solvent heater; Be respectively arranged with valve between the solution inlet of these two crystallization kettles and solution inlet and contact, also be respectively arranged with valve between supercritical fluid inlet and supercritical fluid inlet and contact; The outlet of these two crystallization kettles is connected in parallel respectively, forms outlet and contact; Outlet and contact are communicated with the decompressor inlet; Be respectively arranged with valve between the outlet of these two crystallization kettles and outlet and contact.
3. according to claim 1 and 2ly prepare the typical process flow of superfine powder, it is characterized in that, between each equipment, set up measurement, control instrument and valve with the supercritical fluid anti-solvent process; Valve in this basic procedure can be manual, also can be automatic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310120867 CN1257758C (en) | 2003-12-26 | 2003-12-26 | Basic process flow for preparing superfine powder using supercritical fluid reverse solvent process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310120867 CN1257758C (en) | 2003-12-26 | 2003-12-26 | Basic process flow for preparing superfine powder using supercritical fluid reverse solvent process |
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| Publication Number | Publication Date |
|---|---|
| CN1554463A true CN1554463A (en) | 2004-12-15 |
| CN1257758C CN1257758C (en) | 2006-05-31 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200310120867 Expired - Fee Related CN1257758C (en) | 2003-12-26 | 2003-12-26 | Basic process flow for preparing superfine powder using supercritical fluid reverse solvent process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295006C (en) * | 2005-04-21 | 2007-01-17 | 上海大学 | Method of preparing dragon's blood ultrafine powder using super crifical fluid reverse solvent method |
| CN101474492B (en) * | 2008-12-23 | 2011-03-16 | 南京师范大学 | Method and equipment for preparing super fine powder using ceramic film antisolvent coupling process in semi-continuous type |
| CN104931647A (en) * | 2015-04-09 | 2015-09-23 | 青岛科技大学 | Dynamical quick measuring device for desolventizing residual solvent in thermosensitive solid medicine in high-pressure CO2 (carbon dioxide) manner |
| CN108310797A (en) * | 2018-04-09 | 2018-07-24 | 南通市华安超临界萃取有限公司 | A kind of supercritical fluid recrystallization device |
| CN108409821A (en) * | 2018-03-19 | 2018-08-17 | 青岛国海生物制药有限公司 | A kind of preparation method and megestrol acetate of megestrol acetate nanocrystal |
| CN114699793A (en) * | 2022-05-17 | 2022-07-05 | 黄河水利职业技术学院 | Anti-scaling crystallization equipment capable of continuously discharging |
-
2003
- 2003-12-26 CN CN 200310120867 patent/CN1257758C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295006C (en) * | 2005-04-21 | 2007-01-17 | 上海大学 | Method of preparing dragon's blood ultrafine powder using super crifical fluid reverse solvent method |
| CN101474492B (en) * | 2008-12-23 | 2011-03-16 | 南京师范大学 | Method and equipment for preparing super fine powder using ceramic film antisolvent coupling process in semi-continuous type |
| CN104931647A (en) * | 2015-04-09 | 2015-09-23 | 青岛科技大学 | Dynamical quick measuring device for desolventizing residual solvent in thermosensitive solid medicine in high-pressure CO2 (carbon dioxide) manner |
| CN108409821A (en) * | 2018-03-19 | 2018-08-17 | 青岛国海生物制药有限公司 | A kind of preparation method and megestrol acetate of megestrol acetate nanocrystal |
| CN108310797A (en) * | 2018-04-09 | 2018-07-24 | 南通市华安超临界萃取有限公司 | A kind of supercritical fluid recrystallization device |
| CN114699793A (en) * | 2022-05-17 | 2022-07-05 | 黄河水利职业技术学院 | Anti-scaling crystallization equipment capable of continuously discharging |
| CN114699793B (en) * | 2022-05-17 | 2023-06-23 | 黄河水利职业技术学院 | Anti-scaling crystallization equipment capable of continuously discharging |
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| Publication number | Publication date |
|---|---|
| CN1257758C (en) | 2006-05-31 |
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