CN106563286B - A kind of overcritical atomization crystallization processes preparation receives micron particles and crystallizes hanging basket - Google Patents
A kind of overcritical atomization crystallization processes preparation receives micron particles and crystallizes hanging basket Download PDFInfo
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- CN106563286B CN106563286B CN201610969720.8A CN201610969720A CN106563286B CN 106563286 B CN106563286 B CN 106563286B CN 201610969720 A CN201610969720 A CN 201610969720A CN 106563286 B CN106563286 B CN 106563286B
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- hanging basket
- crystallization
- filter paper
- overcritical
- micron particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0027—Evaporation of components of the mixture to be separated by means of conveying fluid, e.g. spray-crystallisation
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Abstract
Micron particles, which are received, the present invention relates to a kind of overcritical atomization crystallization processes preparation crystallizes hanging basket, mainly solve it is existing based on technology using there is vortex in hanging basket when common straight barrel type crystallization hanging basket, the technical problems such as crystal has diauxie, and the average particle size prepared is big, size distribution area is wide, the particle rate of recovery is relatively low.The present invention includes inner cavity from top to bottom successively by coaxial crystallization kettle top cover bonding pad, cylindrical spout rest area, the big downward conical jet area of mouth, the cylinder that cylindrical dry section and cylindrical particle collecting region are formed, multiple layers of filters, bottom cover, it is vortexed with eliminating, eliminate particle diauxic growth, the effects of mutually being collided between reduction particle, the particle prepared has average particle size small, particle distribution area is narrow, the advantages that crystal morphology is complete, the rate of recovery of common hanging basket is promoted to 98% by 76%, improve the safety of Energetic Nanomaterials preparation system, cleaning cost is saved.
Description
Technical field
The present invention relates to prepare nano and micro materials engineering device technique field using supercritical fluid, and in particular to one kind is super to face
Boundary atomization crystallization processes preparation receive micron particles crystallize hanging basket, can be applied to energetic material, medicine, food, cosmetics, material
The preparation field of the superfine powders such as material, industry.
Background technique
The fine research of energetic material is an important topic of academia all the time, and fine can solve existing
Problems existing for explosive such as reduce sensitivity and improve safety, and energization rate of release is more also easy to produce steady detonation, no
The advantages that explosive of one-size is collocated with each other, and improves degree of packing is numerous.
Supercritical fluid carbon dioxide anti-solvent recrystallization method is a kind of ultrafine dust preparation side risen in recent years
Method.Since carbon dioxide is green and pollution-free, super critical condition is easier to realize (31.4 DEG C of temperature, pressure 7.38MPa),
Carbon dioxide under super critical condition has the solubility being close with liquid and the close mobility of gas phase, surface tension
It is zero equal various features, is more advantageous to the preparation of superfine powder.
Overcritical atomization crystallization processes are a kind of technique that supercritical fluid technique prepares smaller particle size particle, and use is this
When method prepares super-fine material, solution is sprayed into crystallization hanging basket through nozzle atomization and is crystallized, the size of crystalline particle in addition to nozzle
Atomization ability it is directly related outer, the flowing law of fluid is also an important factor for influencing crystal size and pattern in hanging basket.
Currently, the structure of crystallization hanging basket is based on tubular, nozzle is coaxial with hanging basket, and fluid-mixing is sprayed from jet expansion high speed
Enter hanging basket, since discontinuity equalization generates vortex, crystal particles are rotated with vortex, when crystal particles move to nozzle exit
When, accelerated by high-speed jet impact, mutually collided between crystal, Crystal Breakup is caused to keep pattern impaired；Meanwhile in inlet zone
Droplet is got on crystallized particle, and droplet is merged with crystal makes crystal that diauxic growth occur, and becomes big granularity crystal.With
The process of the rotation of vortex, crystal fragmentation and diauxic growth is in cycles.The density of crystal particles is bigger in hanging basket, is vortexed rotation
Speed is faster, collides higher with the probability of fusion growth.So hanging basket fluid movement rule to the pattern of crystalline particle and
Granularity has large effect.
Fluid motion rule in hanging basket is mainly influenced by its structure, by optimizing the structure of hanging basket, makes hanging basket inside stream
Body stress equalization can avoid vortex and be formed, promotes the sedimentation of crystalline particle, and the collision for reducing particle inhibits crystal to grow up.It is excellent
The structure for changing hanging basket is the effective way for improving crystalline quality, reducing grain size number.
Summary of the invention
In order to prepare the particle that pattern is complete, distributed area is narrow, it is necessary to avoid vortex in hanging basket from generating, between reduction particle
Collision, inhibit crystal grow up.This invention address that realizing following purpose:
Primary and foremost purpose is to realize that fluid is flowed towards the same direction in hanging basket, avoids vortex from being formed, thus between reducing particle
Collision probability, promote particle precipitation, avoid crystal particles from being influenced diauxic growth by subsequent droplet.
It is another object of the present invention to keep crystalline particle sufficiently dry during the motion, stick to each other shape after sedimentation is avoided
Agglomerates.
It is another object of the present invention to improve the rate of recovery, by using the method that three lamellar spacings are filtered, replace traditional hanging basket
Single layer filter structure makes the rate of recovery reach 98%, and particle blocking rate is close to 100%.
To achieve the above object, the technical solution adopted by the present invention is that:
A kind of overcritical atomization crystallization processes preparation receives micron particles and crystallizes hanging basket, including cylinder, bottom cover, sintered sheets and
Composite filter paper, in which: successively put from top to bottom by coaxial crystallization kettle top cover bonding pad, cylindrical spout the inner cavity of the cylinder
The downward conical jet area of area, big mouth, cylindrical dry section and cylindrical particle collecting region composition, the area Qie Shige is set to pass through up and down
Logical, sintered sheets and composite filter paper are located in the inner cavity of bottom cover, and composite filter paper is made to be located at the tops of sintered sheets, and bottom cover is located at cylinder
Lower port.
The overcritical atomization crystallization processes preparation receive micron particles crystallization hanging basket further include it is at least one set of by column casing, burn
The filter layer of sheeting and composite filter paper composition, column casing is located at the lower end of cylinder lumen, and makes the outer wall of column casing and the inner wall of cylinder
It is in close contact, sintered sheets and composite filter paper be located at the upper end of column casing, and composite filter paper is made to be located at the tops of sintered sheets.
The composite filter paper is from top to bottom successively by organic micro porous filtration film layer, glass fibre filter membrane layer, organic micropore
Filter film layer and common qualitative filter paper layer composition.
Organic micro porous filtration film layer is 1 0.2 micron of organic micropore filtering film, and glass fibre filter membrane layer is 2
0.2 micrometer glass fiber filter membrane, common qualitative filter paper layer are 2 0.2 micron of common qualitative filter papers.
The bottom cover is hollow structure, and the upper end bore is greater than lower end bore, and inner wall sets there are two boss, is respectively used to embedding
Enter composite filter paper and sintered sheets.
The internal diameter of the cylinder dry section is less than the internal diameter of cylindrical particle collecting region.
The diameter of the composite filter paper is greater than the internal diameter of cylindrical particle collecting region, plays sealing, support and filtration.
The diameter of the composite filter paper is greater than the internal diameter of bottom cover, plays sealing, support and filtration.
The conical jet area lower port internal diameter is identical as cylindrical dry section internal diameter.
The lower port of the bottom cover and cylinder is connected through a screw thread；It is equipped in the crystallization kettle top cover bonding pad of the cylinder interior
Screw thread, in order to which crystallization kettle top cover is connected through a screw thread.
The crystallization kettle top cover bonding pad of crystallization kettle top cover and cylinder is connected through a screw thread, and nozzle is placed on cylindrical spout placement
In area, the lower end of nozzle is inserted at the top of conical jet area in aperture, and the degree of cone angle and spraying liquid bunch are bored in conical jet area
The degree at angle is identical, to guarantee that fluid flows after nozzle ejection towards same direction, can avoid the formation of vortex；It is set in cylinder
The cylindrical dry section set, in this area, fluid-flow rate is more slow, and crystalline particle can sufficiently be done behind this region
It is dry；Cylindrical particle collecting region is set in cylinder, and the interior diameter in this region is more slightly larger than cylindrical dry section internal diameter, and filter paper can block
At step, convenient for fixed and sealing；The filter layer that multiple groups are made of column casing, sintered sheets and composite filter paper can be sequentially stacked on circle
Cylindrical particle collecting region forms multilayer gap filter layer with the filter layer in bottom cover.
The present invention is atomized crystallization preparation process suitable for supercritical fluid preparation technology.
The invention adopts the above technical scheme, compared with the background art, has the advantage that
1. inner conical inlet zone is arranged in cylinder, forces fluid to flow in the same direction, avoid the formation of vortex；
2. cylindrical dry section is arranged in cylinder, make crystalline particle with sufficiently dry in the slow motion process of fluid；
3. using multiple filtration technology, the particle rate of recovery is made to be promoted to 98% by 76%, particle blocking rate is close to 100%.
Detailed description of the invention
Fig. 1 is combining structure schematic diagram of the invention；
Fig. 2 is the structural schematic diagram of cylinder of the present invention；
Fig. 3 is the structural schematic diagram of bottom cover of the present invention；
Fig. 4 is the top view of Fig. 3；
Fig. 5 is the structural schematic diagram of composite filter paper of the present invention.
Specific embodiment
As depicted in figs. 1 and 2, the preparation of one of the present embodiment overcritical atomization crystallization processes is received micron particles and is crystallized
Hanging basket, including cylinder 1, bottom cover 2, sintered sheets 3 and composite filter paper 4, in which: the inner cavity of the cylinder 1 is from top to bottom successively by same
The downward conical jet area 103 of the crystallization kettle top cover bonding pad 101 of axis, cylindrical spout rest area 102, big mouth, cylindrical stem
Dry area 104 and cylindrical particle collecting region 105 form, and up and down, sintered sheets 3 and composite filter paper 4 are located at bottom cover 2 in the area Qie Shige
Inner cavity in, and composite filter paper 4 is made to be located at the tops of sintered sheets 3, bottom cover 2 is located at the lower port of cylinder 1 and is connected through a screw thread,
It is connected through a screw thread in the crystallization kettle top cover bonding pad 101 of the cylinder 1 with crystallization kettle top cover.
It further includes two groups by column casing 5, sintering that micron particles crystallization hanging basket is received in the overcritical atomization crystallization processes preparation
The filter layer that piece 3 and composite filter paper 4 form, the sintered sheets 3 and composite filter paper 4 of every group of filter layer are located at the upper end of column casing 5, and make
Composite filter paper 4 is located at the top of sintered sheets 3, and two groups of filter layers are located at the lower end of 1 inner cavity of cylinder from top to bottom, and make two groups of filterings
The outer wall of the column casing 5 of layer and the inner wall of cylinder 1 are in close contact,
As shown in figure 5, the composite filter paper 4 is from top to bottom successively by 1 0.2 micron organic micro porous filtration film layer 401,2
It is commonly fixed to open 0.2 micrometer glass fiber filtering 402,1 0.2 micron of film layer, 0.2 micron of organic micro porous filtration film layer 401 and 2
Property filter paper layer 403 form, to increase crystal particles by when resistance, promote crystal particles be deposited on surface, to mention
High-recovery.
As shown in Figure 3 and Figure 4, the bottom cover 2 is hollow structure, and the upper end bore is greater than lower end bore, and inner wall is equipped with two
A boss 201,202 is respectively used to insertion composite filter paper 4 and sintered sheets 3.
The internal diameter of the cylinder dry section 104 is less than the internal diameter of cylindrical particle collecting region 105, generates one in its inner wall
A boss is tightly pressed against composite filter paper edge at boss, seals.
The diameter of the composite filter paper 4 is greater than the internal diameter of cylindrical particle collecting region 105, plays sealing, support and filtering and makees
With.
The diameter of the composite filter paper 4 is greater than the internal diameter of bottom cover 2, plays sealing, support and filtration.
The 103 lower port internal diameter of conical jet area is identical as cylindrical 104 internal diameter of dry section, makes the inner conical area of hanging basket
The smooth excessiveness between dry section avoids fluid motion from generating vortex to being obstructed at this time.
Using overcritical atomization crystallization processes, the process of micron particles is received using present invention preparation are as follows: fluid-mixing is from spray
Mouth outlet high speed sprays into conical jet area 103, and speed is gradually slack-off during moving downward, and nucleus is formed inside droplet and life
It is long, generate great number of grains and moved downwardly together with fluid, into cylindrical dry section 104 in after, crystal grain prolongs straight line and delays downwards
Slow to move, without obvious mechanicals efforts between crystal in motion process, the solvent of plane of crystal is extracted simultaneously by SCF during the motion
It is dry, when crystal grain reaches first group of filter layer, it is deposited in 4 surface of first layer composite filter paper, SCF entrapment solvent continues through filter paper
It moves downward, granularity lesser crystal grain in part is deposited to second layer composite filter paper 4 or third layer after penetrating first layer composite filter paper 4
4 surface of composite filter paper.It in preparation process, is generated inside cylinder 1 without vortex, after Crystallization between linear downward motion, crystal
Without sharp impacts, the diauxie of no crystal, thus the crystal average particle size being prepared is smaller, particle size distribution is more
Narrow, multilayer filter structure makes the rate of recovery of micron-particle be promoted to 98% by the 76% of common hanging basket, improves energetic material
The safety of refining system, while also saving cleaning cost.
Claims (9)
1. a kind of overcritical atomization crystallization processes preparation receives micron particles and crystallizes hanging basket, including cylinder (1), bottom cover (2), it is sintered
Piece (3) and composite filter paper (4), it is characterised in that: the inner cavity of the cylinder (1) is from top to bottom successively by coaxial crystallization kettle top cover
The downward conical jet area (103) of bonding pad (101), cylindrical spout rest area (102), big mouth, cylindrical dry section (104)
It is formed with cylindrical particle collecting region (105), up and down, sintered sheets (3) and composite filter paper (4) are located at bottom cover in the area Qie Shige
(2) in inner cavity, and composite filter paper (4) is made to be located at the tops of sintered sheets (3), bottom cover (2) is located at the lower port of cylinder (1), institute
The degree for stating conical jet area (103) interior cone angle is identical as the degree of spraying liquid bunch cone angle；The overcritical atomization crystallization processes
It further includes at least one set of being made of column casing (5), sintered sheets (3) and composite filter paper (4) that micron particles crystallization hanging basket is received in preparation
Filter layer, column casing (5) are located at the lower end of cylinder (1) inner cavity, and are in close contact the outer wall of column casing (5) and the inner wall of cylinder (1),
Sintered sheets (3) and composite filter paper (4) are located at the upper end of column casing (5), and composite filter paper (4) is made to be located at the tops of sintered sheets (3).
2. micron particles crystallization hanging basket is received in the overcritical atomization crystallization processes preparation of one kind according to claim 1, spy
Sign is: the composite filter paper (4) is from top to bottom successively by organic micro porous filtration film layer (401), glass fibre filter membrane layer
(402), organic micro porous filtration film layer (401) and common qualitative filter paper layer (403) composition.
3. micron particles crystallization hanging basket is received in the overcritical atomization crystallization processes preparation of one kind according to claim 2, spy
Sign is: organic micro porous filtration film layer (401) is 1 0.2 micron of organic micropore filtering film, glass fibre filter membrane layer
It (402) is 2 0.2 micrometer glass fiber filter membranes, common qualitative filter paper layer (403) is 2 0.2 micron of common qualitative filter papers.
4. micron particles crystallization hanging basket is received in the overcritical atomization crystallization processes preparation of one kind according to claim 3, spy
Sign is: the bottom cover (2) be hollow structure, the upper end bore be greater than lower end bore, inner wall set there are two boss (201,
202) insertion composite filter paper (4) and sintered sheets (3), are respectively used to.
5. micron particles crystallization hanging basket is received in the overcritical atomization crystallization processes preparation of one kind according to claim 4, spy
Sign is: the internal diameter of the cylinder dry section (104) is less than the internal diameter of cylindrical particle collecting region (105).
6. micron particles crystallization hanging basket is received in the overcritical atomization crystallization processes preparation of one kind according to claim 5, spy
Sign is: the diameter of the composite filter paper (4) is greater than the internal diameter of cylindrical particle collecting region (105), plays sealing, support and filtering
Effect.
7. micron particles crystallization hanging basket is received in the overcritical atomization crystallization processes preparation of one kind according to claim 6, spy
Sign is: the diameter of the composite filter paper (4) is greater than the internal diameter of bottom cover (2), plays sealing, support and filtration.
8. micron particles crystallization hanging basket is received in the overcritical atomization crystallization processes preparation of one kind according to claim 7, spy
Sign is: conical jet area (103) the lower port internal diameter is identical as cylindrical dry section (104) internal diameter.
9. the overcritical atomization crystallization processes preparation of one kind according to claim 1-8 is received micron particles and is hung with crystallizing
Basket, it is characterised in that: the bottom cover (2) and the lower port of cylinder (1) are connected through a screw thread；Crystallization kettle in the cylinder (1)
Top cover bonding pad (101) is equipped with internal screw thread, in order to which crystallization kettle top cover is connected through a screw thread.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610969720.8A CN106563286B (en) | 2016-11-03 | 2016-11-03 | A kind of overcritical atomization crystallization processes preparation receives micron particles and crystallizes hanging basket |
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| CN201610969720.8A CN106563286B (en) | 2016-11-03 | 2016-11-03 | A kind of overcritical atomization crystallization processes preparation receives micron particles and crystallizes hanging basket |
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| CN106563286B true CN106563286B (en) | 2019-04-05 |
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| CN112357908A (en) * | 2020-11-12 | 2021-02-12 | 江西铜业技术研究院有限公司 | Continuous preparation device and process for single-walled carbon nanotubes |
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| CN1528505A (en) * | 2003-10-10 | 2004-09-15 | 大连理工大学 | Crystallizing kettle for preparing superfine powder using supercritical anti-solvent process |
| CN1178739C (en) * | 2001-10-17 | 2004-12-08 | 北京伯联纳米科技有限公司 | High-pressure reactor for making nano material by ultracritical crystallization process |
| CN2699969Y (en) * | 2004-04-21 | 2005-05-18 | 浙江大学 | Minitype spray drying device for laboratry |
| TW200621308A (en) * | 2004-12-31 | 2006-07-01 | Metal Ind Res & Dev Ct | Method for producing microparticle by using supercritical fluid and apparatus thereof |
| CN102529376A (en) * | 2010-12-16 | 2012-07-04 | 财团法人金属工业研究发展中心 | Nozzle device and flow dividing element for nozzle device |
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2016
- 2016-11-03 CN CN201610969720.8A patent/CN106563286B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000075281A2 (en) * | 1999-06-09 | 2000-12-14 | University Technology Corporation | Supercritical fluid-assisted nebulization and bubble drying |
| CN1178739C (en) * | 2001-10-17 | 2004-12-08 | 北京伯联纳米科技有限公司 | High-pressure reactor for making nano material by ultracritical crystallization process |
| CN1528505A (en) * | 2003-10-10 | 2004-09-15 | 大连理工大学 | Crystallizing kettle for preparing superfine powder using supercritical anti-solvent process |
| CN2699969Y (en) * | 2004-04-21 | 2005-05-18 | 浙江大学 | Minitype spray drying device for laboratry |
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