CN1178739C - High-pressure reactor for making nano material by ultracritical crystallization process - Google Patents
High-pressure reactor for making nano material by ultracritical crystallization process Download PDFInfo
- Publication number
- CN1178739C CN1178739C CNB011365463A CN01136546A CN1178739C CN 1178739 C CN1178739 C CN 1178739C CN B011365463 A CNB011365463 A CN B011365463A CN 01136546 A CN01136546 A CN 01136546A CN 1178739 C CN1178739 C CN 1178739C
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- screen pack
- filter
- nano material
- autoclave
- overcritical
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- 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
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Abstract
The present invention relates to a high-pressure kettle for preparing micro nanometer materials by a supercritical crystallization method. The high-pressure kettle comprises a kettle body, a coaxial nozzle and a collector for obtaining micro nanometer particles of different sieve meshes, wherein the collector comprises multistage filters; the multistage filters are mutually matched and connected into a whole from top to bottom; the filter on the topmost stage is floated on the support table of the inner wall of the kettle body; the multistage filters can be dismounted, and the filter screen forms upwards projected hemispherical shape. Therefore, the high-pressure kettle has the advantages of acquirement of the micro nanometer particles of the different sieve meshes and convenient operation and has the advantages for lightening the blockage of the micro nanometer particles to the filters, being favorable to satisfaction of the requirements for nanometer materials of different particle diameters and improving the recovery, the quality and the yield of the nanometer materials.
Description
Technical field:
The present invention relates to a kind of autoclave, particularly relate to a kind of overcritical crystallisation and make the autoclave that micro Nano material is used.
Background technology:
The classical production process of micro Nano material has methods such as spray-drying, jet milled, freezing pulverizing, chemical back washing agent and molten gel.More than these methods its characteristics are respectively arranged.The end of the eighties is by the fast expanding supercritical solution method of U.S. scientist invention and become the best method of the organic micro-nano granules of current manufacturing the beginning of the nineties through the super-critical anti extraction of state scientists such as Korea Spro, U.S. development.More than two kinds of methods be referred to as overcritical crystallisation.But, capital equipment one autoclave of using supercritical methanol technology manufacturing micro Nano material is unsatisfactory, gatherer in this autoclave has only grade one filter, and the grading curve of the micro-nano particulate that it obtains is very wide, can not satisfy the needs of people to the micro-nano particulate of difference screening.
Summary of the invention:
The objective of the invention is to overcome the above-mentioned shortcoming of prior art, provide a kind of overcritical crystallisation that can obtain the micro-and nano-particles of different screenings to make the autoclave that micro Nano material is used.
For achieving the above object, the autoclave that the overcritical crystallisation manufacturing of the present invention micro Nano material is used comprises kettle, coaxial nozzle and gatherer, described gatherer is made up of multistage filter, multistage filter is worked in coordination and is fused up and down, and the filter of upper level is floating to be placed on the saddle of inner wall of kettle.
As optimization, described multistage filter is a secondary filter.
As optimization, described multistage filter is a tertiary filter.
As optimization, described multistage filter connects together by screw thread successively.
As optimization, described filter comprises pedestal, screen pack and locking cap.
As optimization, described screen pack is positioned at the locking cap inboard, and this locking cap is fixed on screen pack by screw thread the below of pedestal.
As optimization, described screen pack is the hemisphere face shape that protrude at the center.
As optimization, described multistage filter is followed successively by coarse filter, middle filtrator and fine filtrator from top to bottom.
As optimization, the aperture of the screen pack of described coarse filter is 2 μ m, and the aperture of the screen pack of middle filtrator is 0.2 μ m, and the aperture of the screen pack of fine filtrator is 0.05 μ m.
As optimization, described kettle upper end outer wall is shaped on groove, this groove is built-in with clip, this clip and the retainer ring that is anchored on its periphery are fixed on the kettle upper end with kettle cover, be equipped with sealing ring between kettle cover and the inner wall of kettle, the catch of sealing ring is equipped with in the kettle cover lower end, and coaxial nozzle is installed in the kettle cover center by screw thread; Described filter comprises pedestal, screen pack and locking cap, and this locking cap is fixed on screen pack by screw thread the below of pedestal; Described screen pack is formed by the nickel powder compacting, and described screen pack is a hemisphere face shape protruding upward; The aperture of the screen pack of described multistage filter dwindles from top to bottom successively, and this multistage filter connects together by screw thread, and upper level filter is placed on the boss of kettle upper inner by O-ring gasket is floating.
After adopting technique scheme, autoclave of the present invention can be used for the generation and the collection of micro-and nano-particles, after the micro-and nano-particles that forms by coaxial nozzle sprays in the still, collect the micro-and nano-particles that can obtain different screenings through multistage filter, filtrate filtered is discharged by the relief hole of autoclave body bottom.
After adopting technique scheme, the autoclave that the overcritical crystallisation manufacturing of the present invention micro Nano material is used has following advantage: the micro-and nano-particles that can obtain different screenings, the particle diameter of minimum micro-and nano-particles is less than 50 nanometers, help like this satisfying to the needs of different-grain diameter nano material and the yield and the quality of raising nano material.Handled easily, used multistage filter is detachable, and both available secondary is also available multistage.Used screen pack adopts hemisphere face shape, can alleviate micro-and nano-particles to the obstruction of filter and the output of increase nano material.
Description of drawings:
Fig. 1 is the cutaway view that the overcritical crystallisation of the present invention is made the autoclave that micro Nano material uses:
Fig. 2 is the cutaway view that the overcritical crystallisation of the present invention is made the autoclave screen pack that micro Nano material uses.
The invention will be further described below in conjunction with accompanying drawing:
The overcritical crystallisation of the present invention is made the gatherer 3 that autoclave that micro Nano material uses comprises kettle 1, coaxial nozzle 2, is made up of tertiary filter; Described kettle 1 upper end outer wall is shaped on groove, this groove is built-in with clip 7, this clip 7 and the retainer ring 8 that is anchored on its periphery are fixed on kettle 1 upper end with kettle cover 9, be equipped with sealing ring 10 between kettle cover 9 and kettle 1 inwall, the catch 11 of sealing ring 10 is equipped with by screw thread in kettle cover 9 lower ends, and coaxial nozzle 2 is installed in kettle cover 9 centers by screw thread; Described filter comprises pedestal 4, screen pack 5 and locking cap 6, and this locking cap 6 is fixed on screen pack 5 by screw thread the below of pedestal 4; Described screen pack 5 is formed by the nickel powder compacting, and described screen pack 5 is a hemisphere face shape protruding upward; The aperture of the screen pack 5 of described tertiary filter is followed successively by 2 μ m, 0.2 μ m and 0.05 μ m from top to bottom, and this tertiary filter connects together by the screw thread on its pedestal 4, and upper level filter is placed on the boss of kettle 1 upper inner by O-ring gasket is floating; The top and the bottom of kettle 1 are linked together by weld seam 12, and kettle 1 lower end is shaped on relief hole 13, and this relief hole 13 is used for external pipe.
The specification requirement of the autoclave that the overcritical crystallisation manufacturing of the present invention micro Nano material is used is:
(1) makes test and examination by GB150-89 " GB150-1998 ".
(2) welding line is pressed DV among the HG17-89
3Form, welding rod model are A132.
(3) nondestructive inspection 100%, and the II level that meets among the JB4730-94 is qualified.
(4) after the completion of processing, do the water pressure test with 40Mpa in the still.
(5) design pressure 32Mpa, operating temperature＜80 ℃.
Claims (10)
1, a kind of overcritical crystallisation is made the autoclave that micro Nano material is used, it comprises kettle (1), coaxial nozzle (2) and gatherer (3), it is characterized in that described gatherer (3) is made up of multistage filter, multistage filter is worked in coordination and is fused up and down, and the filter of upper level is floating to be placed on the saddle of kettle (1) inwall.
2, overcritical crystallisation according to claim 1 is made the autoclave that micro Nano material is used, and it is characterized in that described multistage filter is a secondary filter.
3, overcritical crystallisation according to claim 1 is made the autoclave that micro Nano material is used, and it is characterized in that described multistage filter is a tertiary filter.
4, overcritical crystallisation according to claim 1 is made the autoclave that micro Nano material is used, and it is characterized in that described multistage filter connects together by screw thread successively.
5, overcritical crystallisation according to claim 1 is made the autoclave that micro Nano material is used, and it is characterized in that described filter comprises pedestal (4), screen pack (5) and locking cap (6).
6, overcritical crystallisation according to claim 4 is made the autoclave that micro Nano material is used, and it is characterized in that described screen pack (5) is positioned at locking cap (6) inboard, and this locking cap (6) is fixed on screen pack (5) by screw thread the below of pedestal (4).
7, overcritical crystallisation according to claim 6 is made the autoclave that micro Nano material is used, and it is characterized in that the hemisphere face shape that described screen pack (5) protrudes for the center.
8, overcritical crystallisation according to claim 1 is made the autoclave that micro Nano material is used, and it is characterized in that described multistage filter is followed successively by coarse filter, middle filtrator and fine filtrator from top to bottom.
9, overcritical crystallisation according to claim 1 is made the autoclave that micro Nano material is used, the aperture that it is characterized in that the screen pack (5) of described coarse filter is 2 μ m, the aperture of the screen pack of middle filtrator (5) is 0.2 μ m, and the aperture of the screen pack of fine filtrator (5) is 0.05 μ m.
10, overcritical crystallisation according to claim 1 is made the autoclave that micro Nano material is used, it is characterized in that described kettle (1) upper end outer wall is shaped on groove, this groove is built-in with clip (7), this clip (7) and the retainer ring (8) that is anchored on its periphery are fixed on kettle (1) upper end with kettle cover (9), be equipped with sealing ring (10) between kettle cover (9) and kettle (1) inwall, coaxial nozzle (2) is installed in kettle cover (9) center by screw thread; Described filter comprises pedestal (4), screen pack (5) and locking cap (6), and this locking cap (6) is fixed on screen pack (5) by screw thread the below of pedestal (4); Described screen pack (5) is formed by the nickel powder compacting, and described screen pack (5) is a hemisphere face shape protruding upward; The aperture of the screen pack of described multistage filter (5) dwindles from top to bottom successively, and this multistage filter connects together by screw thread, and upper level filter is placed on the boss of kettle (1) upper inner by O-ring gasket is floating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011365463A CN1178739C (en) | 2001-10-17 | 2001-10-17 | High-pressure reactor for making nano material by ultracritical crystallization process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011365463A CN1178739C (en) | 2001-10-17 | 2001-10-17 | High-pressure reactor for making nano material by ultracritical crystallization process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1358564A CN1358564A (en) | 2002-07-17 |
| CN1178739C true CN1178739C (en) | 2004-12-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011365463A Expired - Fee Related CN1178739C (en) | 2001-10-17 | 2001-10-17 | High-pressure reactor for making nano material by ultracritical crystallization process |
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| Country | Link |
|---|---|
| CN (1) | CN1178739C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115253893A (en) * | 2022-07-25 | 2022-11-01 | 安徽科幂仪器有限公司 | Supercritical carbon dioxide preparation device and method for small amount of nano polar particles |
-
2001
- 2001-10-17 CN CNB011365463A patent/CN1178739C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1358564A (en) | 2002-07-17 |
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