CN102847488A - Device and method for preparing ultrafine powder by supercritical fluid - Google Patents
Device and method for preparing ultrafine powder by supercritical fluid Download PDFInfo
- Publication number
- CN102847488A CN102847488A CN201210380191XA CN201210380191A CN102847488A CN 102847488 A CN102847488 A CN 102847488A CN 201210380191X A CN201210380191X A CN 201210380191XA CN 201210380191 A CN201210380191 A CN 201210380191A CN 102847488 A CN102847488 A CN 102847488A
- Authority
- CN
- China
- Prior art keywords
- supercritical fluid
- heating
- autoclave body
- superfine powder
- heating tube
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a device and method for preparing ultrafine powder by supercritical fluid. The device is composed of an autoclave body, a sealing end cap of the autoclave body, an electric heating pipe, a heating pipe carriage, steel cylinders, a solvent recovering device, a separator, expansion chambers, a temperature control device, a temperature sensor, a casing pipe of the temperature sensor, a guide line leading-out pipe, an exhaust port and a control valve of the exhaust port, wherein an electro-thermal film heating pipe heats in an autoclave; a ring support is arranged at the inner bottom of the autoclave body; the support is fixedly provided with the heating pipe; the heating pipe is connected with the output end of the external temperature control device by a guide line; the sealing end cap is provided with an air port which is simultaneously connected with the solvent recovering device and the steel cylinder trough a guide pipe; and an air port on the side face of the autoclave body is simultaneously connected with another steel cylinder and another expansion chamber through a guide pipe. The device for preparing the ultrathin powder by the supercritical fluid disclosed by the invention is simple to operate, uniform in heating and high in heating speed, can control temperature accurately, can adopt dry ice as a supercritical fluid medium, and can be used for preparing the ultrathin powder and aerogel with nanometre materials simultaneously through a rapid expansion process and a drying process of the supercritical fluid.
Description
Technical field
The present invention relates to the apparatus and method for functional material preparation, particularly relate to and a kind ofly be applicable to utilize the supercritical fluid preparation to comprise the apparatus and method of superfine powder and the aerogel material of nanoscale compound.
Background technology
Superfine powder refers to from micron order to nano level a series of super-fine materials.Because fine size, narrowly distributing, thereby have that specific area is large, surface-active is high, chemical reaction velocity is fast, dissolution velocity is fast, sintered body intensity is large and unique electrically, magnetic, optical etc., be used widely in fields such as material, chemical industry, light industry, metallurgy, electronics, biology, medical science, genetic engineering, sensor manufacturing, health food and military affairs, Aeronautics and Astronautics.Yet superfine powder is because particle diameter is little, and surface area ratio is large, agglomeration easily occurs.Solving agglomeration traits is a large difficult point of superfine powder.
Supercritical fluid (SCF) Technique for Preparing Fine is a new technology that grows up in recent ten years, can produce the ultrafine powder between particle diameter 1～100nm.Utilize SCF Technology in Preparation of Ultrafine Powder to have product purity high, the geometry homogeneous, narrow diameter distribution, particle agglomeration is few; Manufacturing process is simple, and operating temperature is lower, and the suitable material scope is wide etc.This technology has been opened up the new way of preparation ultrafine powder, be particularly suitable for preparing the ultrafine powder with thermal sensitivity, oxidisability, bioactivator, be continue the SCF technology be applied to the extraction, reacted another frontier, be the preparation ultrafine powder a kind of effective means.The supercritical fluid Technique for Preparing Fine is divided into again SCF rapid expanding method (RESS), the anti-solvent method of SCF (SAS) and SCF seasoning (SCFD).
The enforcement of supercritical fluid Technique for Preparing Fine need to have the device that supercritical fluid is provided, and device mainly comprises autoclave, heater, fluid discharge pipe, medium inlet tube.If adopt CO
2Be supercritical fluid, also need pressurized equipment, and the liquid CO 2 conveying equipment, whole apparatus structure is complicated, and cost is high, and is difficult in maintenance.Supercritical fluid often needs HTHP, and heater all is to heat by twining electric furnace heating wire in the kettle outside, because the kettle wall thickness, rate of heat transfer is slower, makes heat time heating time long, and temperature is difficult for stable control, cause preparation cost high, limited the promotion and application of this technology.
Summary of the invention
The present invention is in order to solve above-mentioned super critical fluid apparatus complex structure, heat technical problem slow, that be difficult for temperature control, and propose a kind of simple in structure, easy and simple to handle, rate of heat addition fast, can accurate temperature controlling, be applicable to utilize using supercritical fluid quick expansion method and supercritical fluid drying preparation to comprise supercritical fluid treatment device and the method for superfine powder and the aeroge of nano material.
The present invention is for solving above-mentioned super critical fluid apparatus complex structure, heating is slow, the technical problem that is difficult for temperature control is taked following technical scheme: this device is by autoclave body and end cover thereof, electric heating tube and electrode thereof, the heating tube bracing frame, steel cylinder, solvent recycler, separator, expanding chamber, temperature controller, temperature sensor and sleeve pipe thereof, the wire fairlead, Pressure gauge, exhaust outlet and by-pass valve control thereof form, it is characterized in that: adopt heating in the electrothermal film heating pipe still, the kettle inner bottom part is installed ring support, fixing heating tube on the support, heating tube is connected with outside temperature controller output by wire, have a blow vent to be connected with gas bomb with solvent recycler simultaneously through conduit on the end cover, autoclave body side blow vent is connected with expanding chamber with another gas bomb through conduit simultaneously.
The present invention can also adopt following technical measures:
1. electric heating tube is circular, and the electrothermal tube outside is coated with Electric radiant Heating Film, and Electric radiant Heating Film scribbles insulating protective layer outward.
2. ring support is connected with heating tube and adopts binding agent bonding, leaves the space between at the bottom of heating tube bottom and the still.
3. the Electric radiant Heating Film two end electrodes is connected by the outer temperature controller of wire and kettle.
4. simultaneously with on solvent recycler and the gas conduit that gas bomb is connected by-pass valve control is installed on the end cover.
5. autoclave body side blow vent and steel cylinder are connected with expanding chamber and by-pass valve control are installed on the conduit that is connected.
6. one kind prepares the superfine powder that comprises the nanoscale compound or the method for aeroge: carry out using supercritical fluid quick expansion or supercritical fluid drying for different product, supercritical fluid wherein is the mixing of dry ice, ethanol, acetone, isopropyl alcohol, water or above-mentioned substance.
Adopt technical scheme of the present invention can provide a kind of simple in structure, easy and simple to handle, adopt heating in the Electric radiant Heating Film still, homogeneous heating, the rate of heat addition is fast, operating time is short, energy consumption is low, can accurate temperature controlling, and can be with dry ice as supercritical fluid media, omit the required various device of liquid CO 2, realize simultaneously that on a covering device preparation of using supercritical fluid quick expansion method and supercritical fluid drying comprises the superfine powder of nano material and the supercritical fluid treatment device of aeroge.
Description of drawings
Fig. 1 is the schematic diagram that is used for supercritical fluid treatment device of some embodiments of the present invention.
Fig. 2 is the autoclave schematic diagram for supercritical fluid.
Description of drawings is as follows:
Fig. 1 is described as follows: autoclave body 1, end cover 2, heating tube 3, CO
2Steel cylinder 4, solvent recycler 5, separator 6, expanding chamber 7, nitrogen cylinder 8, temperature controller 9, CO
2 Path control valve 10, solvent recovery pipe-line control valve 11, pressure-control valve 12, nitrogen path control valve 13, expansion fluid control valve 14.
Fig. 2 is described as follows: fastening bolt 15, ring support 16, electrode 17, temperature tube 18, wire fairlead 19, Pressure gauge 20.
The specific embodiment
The invention will be further described below in conjunction with accompanying drawing.
As shown in Figure 1, 2, autoclave body 1 is connected sealing with end cover 2 usefulness fastening bolts 15.CO
2Steel cylinder 4 is connected with pipeline with end cap 2 blow vents, and pipeline is by CO
210 controls of path by-pass valve control open and close; Solvent recycler 5 is connected with end cover 2 usefulness pipelines, and pipeline is opened and closed by 11 controls of solvent recovery pipe-line control valve door.Solvent recycler 5 and CO
2Steel cylinder 4 shares a pipeline and is communicated with the end cover blow vent, and an escape pipe is arranged on the end cap, and setting pressure table 20 on the pipe is by pressure-control valve 12 control still internal pressures.
Nitrogen cylinder 8 is connected with autoclave body 1 usefulness pipeline, is opened and closed by valve 13 controls, and expanding chamber 7 is connected with kettle 1 usefulness pipeline, by valve 14 controls.Expanding chamber 7 shares a pipeline with nitrogen cylinder 8 and is communicated with the kettle blow vent, and expanding chamber 7 is used pipeline connection with separator 6.
Container and pipeline coat the insulation of thermal-insulation heat-resistant material in apparatus of the present invention.
Heating tube 3 is installed in the kettle 1, adds hot fluid to supercriticality, heating tube is pipe, and material adopts glass, pottery or enamel.The ring support 16 that is fixed at the bottom of the still bonds together with electrothermal tube, supports heating tube, makes to leave the slit at the bottom of heating tube and the still and be beneficial to Fluid Flow in A.
The heating tube outer wall is coated with Electric radiant Heating Film, adopts vapour deposition process to plate one deck inorganic nano Electric radiant Heating Film, determines Electric radiant Heating Film resistance according to the heating power size.
The Electric radiant Heating Film two ends scribble the silver slurry, and as electrode, contact conductor is drawn outside the still by the wire fairlead and is connected with temperature controller, and the wire fairlead is filled inorganic ceramic powder and organic adhesion agent composition, pipe end metal nut fit sealing.
The Electric radiant Heating Film outside scribbles one deck insulating protective layer, and the main component of insulating protective layer is polyimide insulated paint.
There is a temperature tube kettle side, and in-built thermocouple is connected on the temperature controller, and temperature controller is selected the commercially available prod, and its panel is provided with thermometer and the Temperature Setting button of reflection autoclave body internal temperature, and temperature control precision is ± 1 ℃.
Below explanation adopts apparatus of the present invention to carry out the workflow of supercritical carbon dioxide drying: wet stock to be processed is packed in the autoclave body 1, add a certain amount of absolute ethyl alcohol, cover end cover 2, make end cap and autoclave body sealed engagement with fastening bolt 15 fit sealings.Open nitrogen path control valve 13 and pressure-control valve 12 in nitrogen cylinder 8 pipelines, pass into the complete rear valve-off of nitrogen replacement air.Open heating power supply, make ethanol reach supercriticality, the insulation certain hour is opened solvent recovery pipe-line control valve 11, emits solvent until discharge fully, opens at last nitrogen path control valve 13, passes into nitrogen, purges product in the complete rear taking-up still.
Below explanation adopts apparatus of the present invention to carry out the workflow of another kind of specific embodiment using supercritical fluid quick expansion method: add first solute in autoclave body 1, and then add a certain amount of drikold, cover end cover 2, make end cap and autoclave body sealed engagement with fastening bolt 15 fit sealings.Open the nitrogen path control valve 13 in nitrogen cylinder 8 pipelines, pass into the complete rear valve-off of nitrogen replacement air.Open heating power supply, make carbon dioxide reach supercriticality, the insulation certain hour, open expansion fluid control valve 14, supercritical fluid is entered in the expanding chamber 7, saturated supercritical fluid is sprayed fast by nozzle, and receive the end product particulate at dash receiver.Solvent enters into separator 6 and reclaims.Open at last CO
2 Path control valve 10 in steel cylinder 4 pipelines passes into CO
2Until solute flows out fully.Separate out in pipeline for fear of solute, must to the pipeline heat tracing, can not separate out at pipeline to guarantee it.
Embodiment 1: the dry preparation of Supercritical Ethanol Al
2O
3Superfine powder
Take by weighing the plan book boehmite of certain mass, will intend first the book boehmite with absolute ethanol washing to displace moisture wherein, obtain Al
2O
3XH
2The alcogel of O.Alcogel is placed supercritical drying device, add an amount of absolute ethyl alcohol as supercritical solvent.The sealing supercritical drying device, logical N
2Purge several minutes with the air in the system of removing, design temperature also begins to heat up.260 ℃ of pressure reach approximately 7.0MPa to treat to rise to temperature approximately, keep this state 1 hour.Then device for opening solvent recovery control valve is slowly emitted extremely solvent-free outflow of solvent wherein, uses at last N
2Purging makes temperature be down to room temperature, opens seal cover and takes out product A l
2O
3Superfine powder.
Embodiment 2: supercritical CO
2Rapid expanding prepares drug powder
Get a certain amount of solid drugs particle, place overcritical still, add an amount of drikold as supercritical solvent.The sealing supercritical drying device, logical N
2Purging is with the air in the system of removing, and design temperature also begins to heat up.50 ℃ of pressure reach approximately 20MPa to treat to rise to temperature approximately, keep this state 1 hour.Then open the expansion fluid control valve and make supercritical fluid solution enter expanding chamber, saturated supercritical fluid sprays fast by nozzle, and receives drug powder at dash receiver.Carbon dioxide enters into separator, uses CO
2Purge until solvent-free outflow.Take out at last the drug powder that makes.
Claims (7)
1. apparatus and method of utilizing supercritical fluid to prepare superfine powder, this device is by autoclave body and end cover thereof, electric heating tube and electrode thereof, the heating tube bracing frame, steel cylinder, solvent recycler, separator, expanding chamber, temperature controller, temperature sensor and sleeve pipe thereof, the wire fairlead, Pressure gauge, exhaust outlet and by-pass valve control thereof form, it is characterized in that: adopt heating in the electrothermal film heating pipe still, at the kettle inner bottom part ring support is installed, fixing heating tube on the support, heating tube is connected with outside temperature controller output by wire, have a blow vent to be connected with gas bomb with solvent recycler simultaneously through conduit on the end cover, autoclave body side blow vent is connected with expanding chamber with another gas bomb through conduit simultaneously.
2. according to claims 1 described device and method that utilizes supercritical fluid to prepare superfine powder, it is characterized in that: electric heating tube is for circular, and the electrothermal tube outside is coated with Electric radiant Heating Film, and Electric radiant Heating Film scribbles insulating protective layer outward.
3. according to claims 1 described device and method that utilizes supercritical fluid to prepare superfine powder, it is characterized in that: ring support is connected with heating tube and adopts binding agent bonding, leaves the space between at the bottom of heating tube bottom and the still.
4. according to claims 1 described device and method that utilizes supercritical fluid to prepare superfine powder, it is characterized in that: the Electric radiant Heating Film two end electrodes is connected by the outer temperature controller of wire and kettle.
5. according to claims 1 described device and method that utilizes supercritical fluid to prepare superfine powder, it is characterized in that: simultaneously with on solvent recycler and the gas conduit that gas bomb is connected by-pass valve control is installed on the end cover.
6. according to claims 1 described device and method that utilizes supercritical fluid to prepare superfine powder, it is characterized in that: autoclave body side blow vent and steel cylinder are connected with expanding chamber and by-pass valve control are installed on the conduit that is connected.
7. one kind prepares the superfine powder that comprises the nanoscale compound or the method for aeroge, described method adopts each described device of claims 1-6 to material handling, it is characterized in that: carry out using supercritical fluid quick expansion or supercritical fluid drying for different product, supercritical fluid wherein is the mixing of dry ice, ethanol, acetone, isopropyl alcohol, water or above-mentioned substance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210380191XA CN102847488A (en) | 2012-10-09 | 2012-10-09 | Device and method for preparing ultrafine powder by supercritical fluid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210380191XA CN102847488A (en) | 2012-10-09 | 2012-10-09 | Device and method for preparing ultrafine powder by supercritical fluid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102847488A true CN102847488A (en) | 2013-01-02 |
Family
ID=47394704
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210380191XA Pending CN102847488A (en) | 2012-10-09 | 2012-10-09 | Device and method for preparing ultrafine powder by supercritical fluid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102847488A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103363783A (en) * | 2013-07-15 | 2013-10-23 | 哈尔滨工业大学 | Supercritical fluid drying device and application method thereof |
| CN105591101A (en) * | 2015-12-15 | 2016-05-18 | 天津斯特兰能源科技有限公司 | Method and device for refining iron phosphate with supercritical fluid expansion technology |
-
2012
- 2012-10-09 CN CN201210380191XA patent/CN102847488A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103363783A (en) * | 2013-07-15 | 2013-10-23 | 哈尔滨工业大学 | Supercritical fluid drying device and application method thereof |
| CN105591101A (en) * | 2015-12-15 | 2016-05-18 | 天津斯特兰能源科技有限公司 | Method and device for refining iron phosphate with supercritical fluid expansion technology |
| CN105591101B (en) * | 2015-12-15 | 2018-07-31 | 天津斯特兰能源科技有限公司 | The method and device of ferric phosphate is refined using supercritical fluid expansion technique |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN203123938U (en) | Supercritical fluid device for preparing micropowder | |
| RU2715711C2 (en) | Multifunctional coating application system and coating application unit for application of washcoat catalytic coating and/or solution onto substrate and methods of application | |
| JP2017519631A5 (en) | ||
| EP2992123A1 (en) | High temperature and high pressure portable gas heater | |
| CN102847488A (en) | Device and method for preparing ultrafine powder by supercritical fluid | |
| ITRM20070105A1 (en) | WATER DISTILLATION SYSTEM FOR INJECTABLE USE | |
| CN203678371U (en) | Device for preparing nano powder by using ultrasonic atomization-microwave pyrolysis combined method | |
| CN105727579A (en) | Low-cost high-efficiency supercritical spray drying method and equipment for slurry | |
| CN105728746A (en) | Preparing method of nano beryllium powder | |
| CN203816243U (en) | Superheated steam spray drying equipment | |
| CN201007596Y (en) | Microwave vacuum spray drying equipment | |
| CN211401969U (en) | Hot gas circulation test system of pressure vessel | |
| CN205582332U (en) | Experimental device for can be used to diagenesis mineralization process simulation | |
| CN103508489A (en) | Nanometer titanium dioxide preparation apparatus and preparation method for nanometer titanium dioxide dioxideby using same | |
| RU2543051C2 (en) | Apparatus for producing strontium-82 | |
| CN102671412B (en) | Sublimation-method pyrogallic acid cold trap recovery device | |
| CN102071034B (en) | Epithermal injection biomass pyrolytic system | |
| JP7266358B2 (en) | Spray fine particle production equipment | |
| CN108680006A (en) | A kind of dewaxing-sintering furnace | |
| CN215234072U (en) | High-pressure reaction tube for fixed bed | |
| CN202239617U (en) | Device for generating aluminum nitride film on surface of spherical aluminum powder by means of microwave radiation | |
| CN220970756U (en) | Alloy powder dehydrogenation furnace | |
| CN107935030A (en) | A kind of method that pyrolytic coating curing prepares strontium titanates coating | |
| CN203572219U (en) | Multifunctional microwave high-temperature experimental furnace | |
| CN208345790U (en) | The manufacture structure of nanometer water |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130102 |